Centrifugal ultrafiltration after methanol extraction of whole plasma was used as an optimal condition for the preparation of blood plasma before metabonomic studies. The plasma samples from 102 lung cancer patients a...Centrifugal ultrafiltration after methanol extraction of whole plasma was used as an optimal condition for the preparation of blood plasma before metabonomic studies. The plasma samples from 102 lung cancer patients and 34 healthy volunteers were prepared with this approach. With ultra-performance liquid chromatography（UPLC） coupled with quadrupole time-of-flight mass spectrometry（Q-TOF MS） analysis, the samples were investigated in order to find potential disease biomarkers. After data acquisition, orthogonal signal correction partial least squares models were built to differentiate the healthy volunteers from lung cancer patients and to identify metabolites that showed significantly different expression between the two groups. Several metabolite ions were identified as potential biomarkers according to the variable importance in the project（VIP） value in both ion modes. Five lysophosphatidylcholines were further identified as specifically lysoPC 16：0, isomer of lysoPC 16：0, lysoPC 18：0, lysoPC 18：1 and lysoPC 18：2. These results suggest that UPLC coupled with Q-TOF MS is an effective technique for the analysis of plasma metabolites in metabonomic studies.展开更多
The residual clothianidin in rice was determined by Agilent ultra-performance liquid chromatography-tandem mass spectrometry, quantified by external standard method, adjusted the elution gradient of mobile phase and t...The residual clothianidin in rice was determined by Agilent ultra-performance liquid chromatography-tandem mass spectrometry, quantified by external standard method, adjusted the elution gradient of mobile phase and the parameters of ion monitoring and analysis, and compared the precision of recovery and repeatability of parallel standard addition. The experimental results showed that the clothianidin residue in rice was ultrasonically extracted by 0.1% acetic acid-acetonitrile and purified by matrix dispersed solid-phase extractant, and the linearity of the test was good. The correlation coefficient R was greater than or equal to 0.999, and the quantitative limit was 0.010mg/kg. The recoveries of clothianidin residue were 96.9% and 95.0% respectively, and the repeatability precision RSD was 1.48%. In this paper, the recovery and precision of parallel standard addition for determination of clothianidin residues in rice by Agilent ultra-performance liquid chromatography-tandem mass spectrometry were studied. Good results were obtained, which could provide reference for the detection of pesticide residues in other cereals.展开更多
In this study, a new technique was developed using rapid ultra-performance liquid chromatography (UPLC)-based separation coupled with electrochemical detection by a boron-doped diamond (BDD) electrode for the detectio...In this study, a new technique was developed using rapid ultra-performance liquid chromatography (UPLC)-based separation coupled with electrochemical detection by a boron-doped diamond (BDD) electrode for the detection and quantification of three commonly used parabens (methylparaben (MP), ethylparaben (EP) and propylparaben (PP)). We aimed to reduce the analysis time by using UPLC coupled with a short reverse phase C 18 monolithic column (25 mm×4.6 mm). Operating the monolithic column at low back-pressure resulted in high flow rates. A mobile phaseconsisting of a 25:75 (v/v) ratio of acetonitrile:0.05 Mphosphate buffer (pH 5) at a flow rate of 2.5 mL·min?1 was used to perform the separation. The amperometric detection with the BDD electrode was found to be optimal and reliably reproducible at a detection potential of 1.5 V vs. Ag/AgCl. Under these conditions, the separation of the three targetanalytes (MP, EP and PP) was achieved in 2 min and was linear within a sample concentration range of 0.1 to 50.0 mg·L?1 (r2 values of 0.9970, 0.9994 and 0.9994 for MP, EP and PP, respectively). This method was successfully applied to determine the concentrations of each parabeninsix real samples with therecoveries ranging from of 80.3% - 98.9% for all three parabensfrom samples spiked at 12, 22 and 32 mg·L?1. Therefore, the proposed method can be used as an alternative rapid and selective method for the determination of paraben levels in real samples.展开更多
OBJECTIVE: To establish a method to analyze the commonalities and characteristics of the aqueous extracts from three Uighur medicines.METHODS: In this study, a combination method of three-stage infrared spectroscopy a...OBJECTIVE: To establish a method to analyze the commonalities and characteristics of the aqueous extracts from three Uighur medicines.METHODS: In this study, a combination method of three-stage infrared spectroscopy and ultra-performance liquid chromatography-time of flight-mass spectra(UPLC-TOF-MS) method was used to analyze the commonalities and characteristics of the aqueous extracts from Hezi(Fructus Chebulae),Maohezi(Terminalia Belliricae Fructus) and Xiqingguo(Chebulae Fructus Immaturus).RESULTS: In Fourier transform-infrared spectroscopy spectra, all three samples showed the characteristic absorption peaks of tannins similarly. According to UPLC-TOF-MS data analysis, the difference of the position and intensity of the peaks at 1713-1707 cm^(-1) in the three samples were related to the difference in the relative content of tannin and pentacyclic triterpenoids. In second derivative infrared spectroscopy spectra, further analysis of the differences in the infrared spectra of the three samples was performed by increasing the apparent resolution. In combination with UPLC-TOF-MS data, some features infrared absorption peaks were assigned.The absorption peaks at 1032-1030 cm^(-1) assigned to the stretching vibration of C-O-C(ether bond)groups of tannins; 1164-1163, 1063-1062, 1009-1005, 904 cm^(-1) attributed to the stretching vibration of C-O(ether bond) and C-O-C groups of glycosidic compounds. 1385-1383 cm^(-1) attributed to the bending vibration of C-H(alkyl hydrogen) of methoxyl group of pentacyclic triterpenoids. Peak 835 cm^(-1) was assigned to the characteristic absorption peak of bending vibration of = C-H groups of pentacyclic triterpenoids. The two dimensional correlation infrared spectroscopy could further quickly distinguish three samples through the dynamic structural information of their chemical components and discrepancy of auto-peaks and cross-peaks intuitively in the range of 1720-419 cm^(-1).CONCLUSION: By comparing the intensity of the infrared characteristic absorption peaks, the main chemical components were assigned, which significantly enriched and perfected the data analysis of the infrared spectra of three Uighur Medicines. It provided a rationale for the identification of medicinal materials with complex and similar chemical components using the three-stage infrared spectroscopy and UPLC-TOF-MS.展开更多
A method was developed for the detection of seven microcystins(microcystin-LR, RR, YR, LA, LY, LW and LF) in surface water using automatic solid-phase extraction(A-SPE) coupled with ultra-performance liquid chromatogr...A method was developed for the detection of seven microcystins(microcystin-LR, RR, YR, LA, LY, LW and LF) in surface water using automatic solid-phase extraction(A-SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). The automated solid-phase extraction system was used to extract microcystins(MCs) from water samples. UPLC-MS/MS was used to determine MCs concentrations in just 5 min. Method detection limits were from 0.3 to 0.9 ng/L, microcystin recoveries ranged from 83.8% to 114%, and the relative standard deviation(RSD) varied from 5.6% to 12.5%. This analytical approach was found to be simple, highly sensitive, accurate, which required little manual operation. Additionally, to validate this analytical method, A-SPE+UPLC-MS/MS was applied to characterize the concentration of MCs in Taihu Lake, Wuxi, China.展开更多
OBJECTIVE:To identify the active ingredients and metabolites in rat bile after Guangtongxiao decoction(GTX)had been administered via the rectal route.METHODS:Drug-containing bile samples were collected via a catheter ...OBJECTIVE:To identify the active ingredients and metabolites in rat bile after Guangtongxiao decoction(GTX)had been administered via the rectal route.METHODS:Drug-containing bile samples were collected via a catheter in the bile duct and could be used 5 h after rectal administration.The main active components and their metabolites in rat bile following rectal administration of GTX were identified and analyzed using ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry.RESULTS:Positive and negative modes were applied to analyze and identify the chemical ingredients in the bioactive fractions of GTX.Eight peaks were identified by comparison with the standard compounds:berberine hydrochloride,dehydrocorydaline,tetrahydropalmatine,corydaline,magnoflorine,magnolol,obacunone and albiflorin.Furthermore,60 metabolites were detected in rat bile based on mass-fragmentation behaviors,and 21 metabolites were reported for the first time.CONCLUSION:Our findings provide a solid basis for further pharmacologic and pharmacokinetic studies of GTX.展开更多
Objective: To compare the pharmacokinetic differences of the main components of Naoxintong capsule(NXTC) in normal and acute blood stasis rats. Materials and Methods: Rats were subcutaneously injected with adrenaline ...Objective: To compare the pharmacokinetic differences of the main components of Naoxintong capsule(NXTC) in normal and acute blood stasis rats. Materials and Methods: Rats were subcutaneously injected with adrenaline hydrochloride twice;during the two subcutaneous injections, the rats were placed in ice water for 4 min to reproduce the model rat of acute blood stasis. The normal and acute blood stasis rats were administrated a 5.04 g/kg dose of NXTC suspension. Then, blood samples were collected from the posterior retinal venous plexus at different time points. Plasma concentrations of four major bio-active components including caffeic acid, ferulic acid, formononetin, and tanshinone IIA in NXTC were measured using ultra-performance liquid chromatography coupled with triple-quadrupole mass spectrometry. Phoenix Win Nonlin v6.2 software was used to calculate the pharmacokinetic parameters. Results: Compared with the normal rats, the acute blood stasis rats showed a significant decrease in C_(max) of ferulic acid and formononetin, AUC_(all) of caffeic acid and ferulic acid, and AUC_(INF_obs) of ferulic acid. Conversely, an increase in the Vz_F_obs and MRT_(last) of ferulic acid and caffeic acid was observed. These findings demonstrate that the absorption of the four NXTC components was weakened in the acute blood stasis rats and that the elimination time was prolonged. Conclusions: The significant difference in some parameters of the four NXTC components between the normal and acute blood stasis rats might be caused by an increase in blood viscosity and the subsequent slowing down of blood flow in the acute blood stasis rats. The pharmacokinetic study conducted in pathological state can provide important information and scientific basis for further rational clinical application of NXTC.展开更多
Objective:There are different geographic origins of Aconiti Kusnezoffii Radixs(AKRs)sold in the market with different quality.This study aims to establish a rapid analysis method to distinguish the different geographi...Objective:There are different geographic origins of Aconiti Kusnezoffii Radixs(AKRs)sold in the market with different quality.This study aims to establish a rapid analysis method to distinguish the different geographic origins of AKRs and to realize the rapid evaluation of their quality.Methods:An ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry(UPLC-Q-TOF MS)method was utilized to acquire the constituents'information of AKRs from different geographic origins.MSE data and Progenesis QI software were employed to identify the chemical constitutes.Principal component analysis(PCA)was applied to comparing MS data to find the chemical markers of AKRs from different geographic origins.Results:Twenty-three components were detected and 17 out of them were identified,including diester-diterpenoid alkaloids,monoester-diterpenoid alkaloids,and amine-diterpenoid alkaloids.Three pairs of isomers were detected and two of them were distinguished by the retention time of standard samples.Thirteen chemical markers were screened out through PCA and orthogonal partial least square discriminant analysis.Through detecting Napelline or isomer of Napelline(m/z 360.2530)and Aconifine(m/z 662.3170),AKRs from inner Mongolia autonomous could be screened.According to the existence of benzoylaconine(m/z 604.3108)and Indaconitine(m/z 630.3159),it could be confirmed that the AKRs are from Xinjiang Uygur autonomous.AKRs that cannot detect compounds above-mentioned could be from Liaoning or Shanxi Province.Conclusions:The chemical profile could be used not only to distinguish the AKRs from different geographic origins but also to identify the true and false of AKRs.This study lays a foundation for the study of efficacy and toxic of AKRs.展开更多
Objective:To study the differences between the serum metabolites in patients with adenomatous polyps of the colon and yang-deficiency constitution and those without colon polyps and with balanced constitution,and look...Objective:To study the differences between the serum metabolites in patients with adenomatous polyps of the colon and yang-deficiency constitution and those without colon polyps and with balanced constitution,and look for biomarkers that can be used to distinguish between the two groups.Methods:General patient information was gathered,and Chinese medicine constitutions were collected in 940 patients who underwent electronic colonoscopy.A total of 119 patients with adenomatous polyps of the colon and yang-deficiency constitution were included in the experimental group,and 150 patients without colon polyps and with balanced constitution were included in the control group.Metabolomics analysis was performed on the fasting venous blood obtained from each patient in both groups.Principal component analysis and orthogonal partial least squares discriminant analysis were performed on the detection results,potential biomarkers were screened,metabolic pathway changes were determined,and the metabolic processes involved were discussed.Results:A total of 59 differential biomarkers between the experimental group and the control group were identified.The differential metabolites were found mainly in the glycerophospholipid metabolism pathway,and the bile acid 3-oxo-4,6-choladienoic acid was the biomarker that distinguished the experimental group from the control group.Conclusions:With the help of metabolomics analysis,the differential metabolites in patients with adenomatous polyps of the colon and yang-deficiency constitution and those in patients without colon polyps and with balanced constitution could be identified.The biomarker 3-oxo-4,6-choladienoic acid may have potential diagnostic value in patients with adenomatous polyp of the colon and yang-deficiency constitution.(Trial Registration No.NCT02986308)展开更多
A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,s...A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,saikosaponin A,and saikosaponin D in rat plasma was developed and validated using butyl p-hydroxybenzoate as an internal standard.One-step direct protein precipitation with acetonitrile was used to extract the compounds from the rat plasma samples.Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)at a flow rate of 0.4 m L/min,using gradient mode containing 0.1%formic acid in water and acetonitrile were used as the Mobile phase A and B.Electrospray ionization in negative ion mode and multiple reaction monitoring were used to identify and quantify active components.Calibration curves showed good linearity(R^2>0.9908)over a wide concentration range for all compounds.The intra-and interday precision(relative standard deviation)ranged 2.4%–7.0%and 2.6%–8.0%,respectively.The accuracy(relative error)was from-13.0%to 13.2%at all quality control levels.The recovery ranged from 81.1%to 92.5%.The validated method was successfully applied to pharmacokinetic study in rats after oral administration of Qing Gan-Shu Yu-Fang.The results show that one can draw a conclusion that these six active ingredients can be quickly absorbed and play a pharmacodynamic role rapidly in vivo.展开更多
Background: Curcuma wenyujin rhizome(CWR) is a commonly used Chinese herbal medicine for treating blood stasis in China for 1000 of years. However, the underlying mechanism of CWR remains unclear. Aims and Objectives:...Background: Curcuma wenyujin rhizome(CWR) is a commonly used Chinese herbal medicine for treating blood stasis in China for 1000 of years. However, the underlying mechanism of CWR remains unclear. Aims and Objectives: The purpose of this study is to clarify the bioactive mechanism of CWR in treating blood stasis. Materials and Methods: In this study, pharmacological indexes, including hemorheology and four blood coagulation indexes were tested. Bile and urine metabolomics were engaged by UPLC-Q/TOF-MS. Multivariate statistical analysis were used to screen out differential endogenous metabolites. Results: The results indicated that CWR significantly ameliorated the hemorheology and coagulation functions of acute blood stasis(ABS) model rats. Moreover, 27 endogenous metabolites between the CWR group and the ABS group were screened, and the levels were all improved to certain degrees by CWR preadministration. Metabonomics results indicated that ABS was mainly related to linoleic acid metabolism, arachidonic acid metabolism, glycerophospholipid metabolism, sphingolipid metabolism, pentose and glucuronate intercereasonversions, steroid hormone biosynthesis, and primary bile acid biosynthesis. Conclusion: In a word, the metabolomics method is consistent with the holistic view of traditional Chinese medicine(TCM) that can be a powerful means to illustrate the biological activity mechanism of CWR in treating blood stasis and to offer research demonstration for further study on the effector mechanism of TCM.展开更多
A high-performance liquid chromatography(HPLC)method has been developed using a CAPCELL PAK ADME(150 mm×4.6 mm,5μm)as analytical column and a gradient elution with 15 min using acetonitrile and 0.1%(in volume fr...A high-performance liquid chromatography(HPLC)method has been developed using a CAPCELL PAK ADME(150 mm×4.6 mm,5μm)as analytical column and a gradient elution with 15 min using acetonitrile and 0.1%(in volume fraction)phosphoric acid water(pH=2.2)as the mobile phase.Three active substances in cosmetics were quantitatively detected simultaneously at a detection wavelength of 265 nm.The linear ranges of β-nicotinamide mononucleotides,ergothioneine and nicotinamide are 10~200 mg/L,5~100 mg/L and 5~100 mg/L respectively and the detection limits of three components are 3.0 mg/L,1.5 mg/L and 1.5 mg/L respectively.The recovery rate is 97.1~104.9%,with RSD≤2.0%.The method was applied to quantitative analysis of five samples of cosmetics toner,lotion,cream,essence and gel and three samples of raw materials.The results showed that the results of β-nicotinamide mononucleotide and ergothioneine in five cosmetics were consistent with the product label,while nicotinamide was inconsistent with the label.The purity of the three raw material samples was 99.5%,99.7% and 100.8%respectively.This method offers high precision,accuracy and short analysis time,making it a reliable approach for studying three active ingredients in cosmetics and suitable for quality control of related functional ingredients.展开更多
Covalent organic frameworks(COFs)have demonstrated great potential in chromatographic separation because of unique structure and superior performance.Herein,single-crystal three-dimensional(3D)COFs with regular morpho...Covalent organic frameworks(COFs)have demonstrated great potential in chromatographic separation because of unique structure and superior performance.Herein,single-crystal three-dimensional(3D)COFs with regular morphology,good monodispersity and high specific surface area,were used as a stationary phase for high-performance liquid chromatography(HPLC).The single-crystal 3D COFs packed column not only exhibits high efficiency in separating hydrophobic molecules involving substituted benzenes,halogenated benzenes,halogenated nitrobenzenes,aromatic amines,aromatic hydrocarbons(PAHs)and phthalate esters(PAEs),but also achieves baseline separation of acenaphthene and acenaphthylene with similar physical and chemical properties as well as environmental pollutants,which cannot be quickly separated on commercial C18 column and a polycrystalline 3D COFs packed column.Especially,the column efficiency of 17303-24255 plates/m was obtained for PAEs,and the resolution values for acenaphthene and acenaphthylene,and carbamazepine(CBZ)and carbamazepine-10,11-epoxide(CBZEP)were 1.7and 2.2,respectively.This successful application not only confirmed the great potential of the singlecrystal 3D COFs in HPLC separation of the organic molecules,but also facilitates the application of COFs in separation science.展开更多
Background:Polygonum multiflorum-induced liver injury(PM-DILI)has significantly hindered its clinical application and development.Methods:This study investigates the variation in content and toxicity of dian-thrones,t...Background:Polygonum multiflorum-induced liver injury(PM-DILI)has significantly hindered its clinical application and development.Methods:This study investigates the variation in content and toxicity of dian-thrones,the toxic components of P.multiflorum,during different processing cycles.We employed the ultra-high-performance liquid chromatography triple quadrupole mass spectrometry method to quantify six dianthrones in raw P.multiflorum and formulations processed with a method called nine cycles of steaming and sunning.Additionally,toxicity assessments were conducted using human normal liver cell line L02 and zebrafish embryos.Results:Results indicate a gradual reduction in dianthrones content with increasing processing cycles.Processed formulations exhibited significantly reduced cytotoxic-ity in L02 cells and hepatotoxicity in zebrafish embryos.Conclusions:Our findings elucidate the relationship between processing cycles and P.multiflorum toxicity,providing theoretical support for its safe use.展开更多
Soil is of particular interest to the forensic community because it can be used as valuable associative evidence to link a suspect to a victim or a crime scene.Liquid chromatography is a powerful analytical tool for o...Soil is of particular interest to the forensic community because it can be used as valuable associative evidence to link a suspect to a victim or a crime scene.Liquid chromatography is a powerful analytical tool for organic compound analysis.Recently,high-performance liquid chromatography(HPLC)has proven to be an efficient method for forensic soil analysis,especially in discriminating soils from proximity locations.However,ultra-performance liquid chromatography(UPLC),which is much more sensitive than HPLC,has never been explored in this context.This study proposed a UPLC method for profiling non-volatile organic compounds in three Malaysian soils(red,brown and yellowish-brown soils).The three soils were analysed separately to assess the effects of individual chromatographic parameters:(a)elution programme(isocratic vs.two gradient programmes);(b)flow rate(0.1 vs.0.2 mL/min);(c)extraction solvent(acetonitrile vs.methanol)and(d)detection wavelength(230 vs.254 nm).The injection volume and total run time were set to 5μL and 35 min,respectively.Consequently,each soil sample gave 24 different chromatograms.Results showed that the most desirable chromatographic parameters were(a)isocratic elution;(b)flow rate at 0.2 mL/min and(c)acetonitrile extraction solvent.The proposed UPLC system is expected to be a feasible method for profiling non-volatile organic compounds in soil,and is more chemical-efficient than a comparable HPLC system.展开更多
Methods for determining nine low molecular weight organic acids in root exudates were developed by using reversed phase high performance liquid chromatography with UV (ultraviolet) detection at 214 nm. The mobile ph...Methods for determining nine low molecular weight organic acids in root exudates were developed by using reversed phase high performance liquid chromatography with UV (ultraviolet) detection at 214 nm. The mobile phase was 18 mmol L -1 kH 2PO 4 adjusted to pH 2.25 with phosphoric acid and the flow rate was 0.3 mL min -1 . The analytical column was a reversed phase silica based C 18 column (Shim pack CLC ODS). The root exudates were collected through submerging the whole root system into aerated deionized water for 2 hours. The filtered exudate solutions were concentrated to dryness by rotary evaporation at 40 °C, dissolved in 10 mL mobile phase. The chromatographic conditions of organic acid determination were analyzed. The results showed that there was a high selectivity and sensitivity in the organic acid determination by reversed phase high performance liquid chromatography. Coefficients of variation for organic acid determination were lower than 10% except lactic acid. The recoveries were consistently between 80.1% to 108.3%. Detection limits were approximately 0.05 to 4.5 mg L -1 for organic acids except succinic acid with the detection limit of 7.0 mg L -1 . Phosphorus deficiency may contribute to the release of organic acids in soybean root exudates especially malic, lactic and citric acids.展开更多
Small peptides have attracted increasing attention for their unique features and diverse biological functions.Achieving rapid separation and accurate quantification,however,remains a challenge because of their low abu...Small peptides have attracted increasing attention for their unique features and diverse biological functions.Achieving rapid separation and accurate quantification,however,remains a challenge because of their low abundance and the co-existence of numerous structural isomers.In this study,we developed a novel approach using isotope chemical labeling for ultrasensitive determination of di/tripeptides in biological samples.We successfully synthesized a novel derivatization reagent,4-(2-(ethoxymethylene)-3-oxobutanamido)-N,N,N-trimethylbenzenaminium iodide(EOTMBA)as well as its deuterium-labeled isotope reagent(d_(3)-EOTMBA).A total of 97 small peptides,including 89 dipeptides and 8 tripeptides,could be completely derivatized in methanol within 1.5h at 60℃.After EOTMBA labeling,analysis of these di/tripeptides were achieved within 22 min by LC-MS/MS analysis.The method demonstrated 86.3%-113%accuracy and the limit of quantification ranged from 0.25 fmol/L to 5 nmol/L.Using this method,we achieved ultrasensitive and accurate quantification of di/tripeptides in 147 plasma,49 urine and 46 bile samples obtained from healthy individuals and patients with biliary tract diseases.The identified differential di/tripeptide biomarker panels showed promising diagnostic performance for patients with biliary tract cancer with area under the receiver operating curve values from 0.870 to 0.996.Furthermore,this method was successfully applied to quantify di/tripeptides in the extract of an animal-derived traditional Chinese medicine,Eupolyphaga sinensis Walker.These findings highlight the possible application of the analytical method in clinics and for the purposes of quality control of traditional Chinese medicines.展开更多
In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Sc...In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Scientific C18 column (250 mm×4.6 mm, 5 μm) as the chromatographic column and acetonitrile and water as the mobile phase, and the excitation wavelength and emission wavelength of fluorescence detector were 286 and 430 nm, respectively. The response was high, and the linear range was 0.5-10.0 ng/ml. The lowest limit of detection was 0.11 ng/ml, and the average recovery was 92.5%. This method is suitable for quantitative analysis of benzo[a]pyrene content in edible oil.展开更多
Carbendazim belongs to the benzimidazole fungicides,which can be used for control lots of fungi pathogens.High-performance liquid chromatography is frequently used for the analysis of carbendazim in all kinds of sampl...Carbendazim belongs to the benzimidazole fungicides,which can be used for control lots of fungi pathogens.High-performance liquid chromatography is frequently used for the analysis of carbendazim in all kinds of samples.In most occasions,the developed methods were applied for the simultaneous detection of a huge number of pesticides.Thus,an analytical method via UPLC-FLD was developed,and the sample preparation process was optimized by studying the effect of extraction solvent,approach,time and purification absorbent on the recovery rate of carbendazim.The results showed the optimized method for analysis was ultrasonication-assisted extraction with acetonitrile for 1 min,and subsequent purification by C18.In this occasion,the established analytical method of carbendazim in tomato samples displayed good linearity,accuracy and precision.展开更多
Aim To establish a reversed-phase liquid chromatographic (LC) method forsimultaneous determination of tetramethylpyrazine (TMP) and aspirin in a new compound formulation.Methods Chromatographic separation of the two d...Aim To establish a reversed-phase liquid chromatographic (LC) method forsimultaneous determination of tetramethylpyrazine (TMP) and aspirin in a new compound formulation.Methods Chromatographic separation of the two drugs was achieved on a Diamonsil C_(18) column, usinga binary mixture of methanol-1.5% acetic acid (35:65, V/V, pH = 3.1) as mobile phase at a flow rateof 1.0 mL·min^(-1). Results Separation was completed in less than 12 min. Benzoic acid was used asthe internal standard. Recoveries at levels corresponding to 80 % to 120 % of the label claim ofthe formulation ranged from 99.6 to 100.3 % for aspirin and from 99.9 to 101.3% for TMP. The linearrange was 12.6 - 150.9 μg·mL^(-1)(r= 0.9997, n = 5) for aspirin and 25.0- 300.0 μg·mL^(-1) (r =0.9999, n = 5) for TMP. Conclusion The method developed can be used for the simultaneousdetermination of TMP and aspirin in pharmaceutical preparations.展开更多
基金Supported by the National Natural Science Foundation of China(No.30801513)the Knowledge Innovation Program of Chinese Academy of Sciences(No.KSCX2-YW-R-170)
文摘Centrifugal ultrafiltration after methanol extraction of whole plasma was used as an optimal condition for the preparation of blood plasma before metabonomic studies. The plasma samples from 102 lung cancer patients and 34 healthy volunteers were prepared with this approach. With ultra-performance liquid chromatography（UPLC） coupled with quadrupole time-of-flight mass spectrometry（Q-TOF MS） analysis, the samples were investigated in order to find potential disease biomarkers. After data acquisition, orthogonal signal correction partial least squares models were built to differentiate the healthy volunteers from lung cancer patients and to identify metabolites that showed significantly different expression between the two groups. Several metabolite ions were identified as potential biomarkers according to the variable importance in the project（VIP） value in both ion modes. Five lysophosphatidylcholines were further identified as specifically lysoPC 16：0, isomer of lysoPC 16：0, lysoPC 18：0, lysoPC 18：1 and lysoPC 18：2. These results suggest that UPLC coupled with Q-TOF MS is an effective technique for the analysis of plasma metabolites in metabonomic studies.
文摘The residual clothianidin in rice was determined by Agilent ultra-performance liquid chromatography-tandem mass spectrometry, quantified by external standard method, adjusted the elution gradient of mobile phase and the parameters of ion monitoring and analysis, and compared the precision of recovery and repeatability of parallel standard addition. The experimental results showed that the clothianidin residue in rice was ultrasonically extracted by 0.1% acetic acid-acetonitrile and purified by matrix dispersed solid-phase extractant, and the linearity of the test was good. The correlation coefficient R was greater than or equal to 0.999, and the quantitative limit was 0.010mg/kg. The recoveries of clothianidin residue were 96.9% and 95.0% respectively, and the repeatability precision RSD was 1.48%. In this paper, the recovery and precision of parallel standard addition for determination of clothianidin residues in rice by Agilent ultra-performance liquid chromatography-tandem mass spectrometry were studied. Good results were obtained, which could provide reference for the detection of pesticide residues in other cereals.
文摘In this study, a new technique was developed using rapid ultra-performance liquid chromatography (UPLC)-based separation coupled with electrochemical detection by a boron-doped diamond (BDD) electrode for the detection and quantification of three commonly used parabens (methylparaben (MP), ethylparaben (EP) and propylparaben (PP)). We aimed to reduce the analysis time by using UPLC coupled with a short reverse phase C 18 monolithic column (25 mm×4.6 mm). Operating the monolithic column at low back-pressure resulted in high flow rates. A mobile phaseconsisting of a 25:75 (v/v) ratio of acetonitrile:0.05 Mphosphate buffer (pH 5) at a flow rate of 2.5 mL·min?1 was used to perform the separation. The amperometric detection with the BDD electrode was found to be optimal and reliably reproducible at a detection potential of 1.5 V vs. Ag/AgCl. Under these conditions, the separation of the three targetanalytes (MP, EP and PP) was achieved in 2 min and was linear within a sample concentration range of 0.1 to 50.0 mg·L?1 (r2 values of 0.9970, 0.9994 and 0.9994 for MP, EP and PP, respectively). This method was successfully applied to determine the concentrations of each parabeninsix real samples with therecoveries ranging from of 80.3% - 98.9% for all three parabensfrom samples spiked at 12, 22 and 32 mg·L?1. Therefore, the proposed method can be used as an alternative rapid and selective method for the determination of paraben levels in real samples.
基金National Science and Technology Major Projects for New Drug Development(No.2017ZX09305005)Scientific Research Funds for High Calibre Researchers of Shihezi University(No.RCSX201715)
文摘OBJECTIVE: To establish a method to analyze the commonalities and characteristics of the aqueous extracts from three Uighur medicines.METHODS: In this study, a combination method of three-stage infrared spectroscopy and ultra-performance liquid chromatography-time of flight-mass spectra(UPLC-TOF-MS) method was used to analyze the commonalities and characteristics of the aqueous extracts from Hezi(Fructus Chebulae),Maohezi(Terminalia Belliricae Fructus) and Xiqingguo(Chebulae Fructus Immaturus).RESULTS: In Fourier transform-infrared spectroscopy spectra, all three samples showed the characteristic absorption peaks of tannins similarly. According to UPLC-TOF-MS data analysis, the difference of the position and intensity of the peaks at 1713-1707 cm^(-1) in the three samples were related to the difference in the relative content of tannin and pentacyclic triterpenoids. In second derivative infrared spectroscopy spectra, further analysis of the differences in the infrared spectra of the three samples was performed by increasing the apparent resolution. In combination with UPLC-TOF-MS data, some features infrared absorption peaks were assigned.The absorption peaks at 1032-1030 cm^(-1) assigned to the stretching vibration of C-O-C(ether bond)groups of tannins; 1164-1163, 1063-1062, 1009-1005, 904 cm^(-1) attributed to the stretching vibration of C-O(ether bond) and C-O-C groups of glycosidic compounds. 1385-1383 cm^(-1) attributed to the bending vibration of C-H(alkyl hydrogen) of methoxyl group of pentacyclic triterpenoids. Peak 835 cm^(-1) was assigned to the characteristic absorption peak of bending vibration of = C-H groups of pentacyclic triterpenoids. The two dimensional correlation infrared spectroscopy could further quickly distinguish three samples through the dynamic structural information of their chemical components and discrepancy of auto-peaks and cross-peaks intuitively in the range of 1720-419 cm^(-1).CONCLUSION: By comparing the intensity of the infrared characteristic absorption peaks, the main chemical components were assigned, which significantly enriched and perfected the data analysis of the infrared spectra of three Uighur Medicines. It provided a rationale for the identification of medicinal materials with complex and similar chemical components using the three-stage infrared spectroscopy and UPLC-TOF-MS.
基金Supported by the Environmental Monitoring and Research Foundation of Jiangsu Province(1621)the Taihu Lake Pollution Prevention and Control Project of Jiangsu Province(TH2016301)Postgraduate Research and Practice Innovation Program of Jiangsu Province in 2016(KYLX16_0813)
文摘A method was developed for the detection of seven microcystins(microcystin-LR, RR, YR, LA, LY, LW and LF) in surface water using automatic solid-phase extraction(A-SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). The automated solid-phase extraction system was used to extract microcystins(MCs) from water samples. UPLC-MS/MS was used to determine MCs concentrations in just 5 min. Method detection limits were from 0.3 to 0.9 ng/L, microcystin recoveries ranged from 83.8% to 114%, and the relative standard deviation(RSD) varied from 5.6% to 12.5%. This analytical approach was found to be simple, highly sensitive, accurate, which required little manual operation. Additionally, to validate this analytical method, A-SPE+UPLC-MS/MS was applied to characterize the concentration of MCs in Taihu Lake, Wuxi, China.
基金Supported by the Youth Program of National Natural Science Foundation of China(To Investigate the Spasmolysis of Intestinal Absorption Solution of Guang Tong Xiao Aqueous Extract&Effective Components for Anal Sphincter Based on Calcium Channels,No.81704077)。
文摘OBJECTIVE:To identify the active ingredients and metabolites in rat bile after Guangtongxiao decoction(GTX)had been administered via the rectal route.METHODS:Drug-containing bile samples were collected via a catheter in the bile duct and could be used 5 h after rectal administration.The main active components and their metabolites in rat bile following rectal administration of GTX were identified and analyzed using ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry.RESULTS:Positive and negative modes were applied to analyze and identify the chemical ingredients in the bioactive fractions of GTX.Eight peaks were identified by comparison with the standard compounds:berberine hydrochloride,dehydrocorydaline,tetrahydropalmatine,corydaline,magnoflorine,magnolol,obacunone and albiflorin.Furthermore,60 metabolites were detected in rat bile based on mass-fragmentation behaviors,and 21 metabolites were reported for the first time.CONCLUSION:Our findings provide a solid basis for further pharmacologic and pharmacokinetic studies of GTX.
基金supported by the National Science and Technology Major Project of China “Key New Drug Creation and Manufacturing Program” 2015ZX09501004-001-007National Natural Science Foundation of China 82004082Top talent training project of TCM in Henan Province。
文摘Objective: To compare the pharmacokinetic differences of the main components of Naoxintong capsule(NXTC) in normal and acute blood stasis rats. Materials and Methods: Rats were subcutaneously injected with adrenaline hydrochloride twice;during the two subcutaneous injections, the rats were placed in ice water for 4 min to reproduce the model rat of acute blood stasis. The normal and acute blood stasis rats were administrated a 5.04 g/kg dose of NXTC suspension. Then, blood samples were collected from the posterior retinal venous plexus at different time points. Plasma concentrations of four major bio-active components including caffeic acid, ferulic acid, formononetin, and tanshinone IIA in NXTC were measured using ultra-performance liquid chromatography coupled with triple-quadrupole mass spectrometry. Phoenix Win Nonlin v6.2 software was used to calculate the pharmacokinetic parameters. Results: Compared with the normal rats, the acute blood stasis rats showed a significant decrease in C_(max) of ferulic acid and formononetin, AUC_(all) of caffeic acid and ferulic acid, and AUC_(INF_obs) of ferulic acid. Conversely, an increase in the Vz_F_obs and MRT_(last) of ferulic acid and caffeic acid was observed. These findings demonstrate that the absorption of the four NXTC components was weakened in the acute blood stasis rats and that the elimination time was prolonged. Conclusions: The significant difference in some parameters of the four NXTC components between the normal and acute blood stasis rats might be caused by an increase in blood viscosity and the subsequent slowing down of blood flow in the acute blood stasis rats. The pharmacokinetic study conducted in pathological state can provide important information and scientific basis for further rational clinical application of NXTC.
基金supported by the National Key Research and Development Project(SQ2018YPC170480,2018YFC1708202)the National Natural Science Foundation of China(81774009)+1 种基金the Key science and technology projects of Inner Mongolia Autonomous Region(2019ZD004)Open Project Program of Inner Mongolia Key Laboratory of Toxicant Monitoring and Toxicology,China(MDK 2019040)。
文摘Objective:There are different geographic origins of Aconiti Kusnezoffii Radixs(AKRs)sold in the market with different quality.This study aims to establish a rapid analysis method to distinguish the different geographic origins of AKRs and to realize the rapid evaluation of their quality.Methods:An ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry(UPLC-Q-TOF MS)method was utilized to acquire the constituents'information of AKRs from different geographic origins.MSE data and Progenesis QI software were employed to identify the chemical constitutes.Principal component analysis(PCA)was applied to comparing MS data to find the chemical markers of AKRs from different geographic origins.Results:Twenty-three components were detected and 17 out of them were identified,including diester-diterpenoid alkaloids,monoester-diterpenoid alkaloids,and amine-diterpenoid alkaloids.Three pairs of isomers were detected and two of them were distinguished by the retention time of standard samples.Thirteen chemical markers were screened out through PCA and orthogonal partial least square discriminant analysis.Through detecting Napelline or isomer of Napelline(m/z 360.2530)and Aconifine(m/z 662.3170),AKRs from inner Mongolia autonomous could be screened.According to the existence of benzoylaconine(m/z 604.3108)and Indaconitine(m/z 630.3159),it could be confirmed that the AKRs are from Xinjiang Uygur autonomous.AKRs that cannot detect compounds above-mentioned could be from Liaoning or Shanxi Province.Conclusions:The chemical profile could be used not only to distinguish the AKRs from different geographic origins but also to identify the true and false of AKRs.This study lays a foundation for the study of efficacy and toxic of AKRs.
文摘Objective:To study the differences between the serum metabolites in patients with adenomatous polyps of the colon and yang-deficiency constitution and those without colon polyps and with balanced constitution,and look for biomarkers that can be used to distinguish between the two groups.Methods:General patient information was gathered,and Chinese medicine constitutions were collected in 940 patients who underwent electronic colonoscopy.A total of 119 patients with adenomatous polyps of the colon and yang-deficiency constitution were included in the experimental group,and 150 patients without colon polyps and with balanced constitution were included in the control group.Metabolomics analysis was performed on the fasting venous blood obtained from each patient in both groups.Principal component analysis and orthogonal partial least squares discriminant analysis were performed on the detection results,potential biomarkers were screened,metabolic pathway changes were determined,and the metabolic processes involved were discussed.Results:A total of 59 differential biomarkers between the experimental group and the control group were identified.The differential metabolites were found mainly in the glycerophospholipid metabolism pathway,and the bile acid 3-oxo-4,6-choladienoic acid was the biomarker that distinguished the experimental group from the control group.Conclusions:With the help of metabolomics analysis,the differential metabolites in patients with adenomatous polyps of the colon and yang-deficiency constitution and those in patients without colon polyps and with balanced constitution could be identified.The biomarker 3-oxo-4,6-choladienoic acid may have potential diagnostic value in patients with adenomatous polyp of the colon and yang-deficiency constitution.(Trial Registration No.NCT02986308)
基金supported financially by the National Natural Science Foundation of China (Grant No. 81973604, 81803690and 81703684)the Innovative Talents Funding of Heilongjiang University of Chinese Medicine(Grant No.2018RCD25)+8 种基金the National natural science foundation matching project (Grant No. 2018PT02)the National natural Science Foundation Matching Project (Grant No. 2017PT01)the Graduate Innovative Research Project Foundation of Heilongjiang University of Chinese Medicine (Grant No. 2019yjscx013)the Postdoctoral Initial Fund of Heilongjiang Provincethe University Nursing Program for Young Scholars with Creative Talents in Heilongjiang Province (Grant No. UNPYSCT2017215 and UNPYSCT2017219)the Natural Science Foundation of Heilongjiang Province (Grant No. H2015037)the Heilongjiang University of Chinese Medicine Doctoral Innovation Foundation (Grant No. 2014bs05)the Application Technology Research and Development Projects of Harbin Technology Bureau (Grant No. 2014RFQXJ149)Heilongjiang Postdoctoral Scientific Research Developmental Fund (Grant No.LBHQ16210 and LBH-Q17161)
文摘A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,saikosaponin A,and saikosaponin D in rat plasma was developed and validated using butyl p-hydroxybenzoate as an internal standard.One-step direct protein precipitation with acetonitrile was used to extract the compounds from the rat plasma samples.Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)at a flow rate of 0.4 m L/min,using gradient mode containing 0.1%formic acid in water and acetonitrile were used as the Mobile phase A and B.Electrospray ionization in negative ion mode and multiple reaction monitoring were used to identify and quantify active components.Calibration curves showed good linearity(R^2>0.9908)over a wide concentration range for all compounds.The intra-and interday precision(relative standard deviation)ranged 2.4%–7.0%and 2.6%–8.0%,respectively.The accuracy(relative error)was from-13.0%to 13.2%at all quality control levels.The recovery ranged from 81.1%to 92.5%.The validated method was successfully applied to pharmacokinetic study in rats after oral administration of Qing Gan-Shu Yu-Fang.The results show that one can draw a conclusion that these six active ingredients can be quickly absorbed and play a pharmacodynamic role rapidly in vivo.
基金financially supported by the National Natural Science Foundation of China (81673598, 81973483, 82003948)Natural Science Foundation of Zhejiang Province (LQ21H280002)+3 种基金The National Key Research and Development Program of China (2018YFC1707000)the National traditional Chinese medicine industry special project (2015468002-2)National Standardization Program for Chinese Medicine (ZYBZH-Y-SC-40)Zhejiang Chinese Medicine University School-level Scientific Research Fund for Talents (2020ZR14)。
文摘Background: Curcuma wenyujin rhizome(CWR) is a commonly used Chinese herbal medicine for treating blood stasis in China for 1000 of years. However, the underlying mechanism of CWR remains unclear. Aims and Objectives: The purpose of this study is to clarify the bioactive mechanism of CWR in treating blood stasis. Materials and Methods: In this study, pharmacological indexes, including hemorheology and four blood coagulation indexes were tested. Bile and urine metabolomics were engaged by UPLC-Q/TOF-MS. Multivariate statistical analysis were used to screen out differential endogenous metabolites. Results: The results indicated that CWR significantly ameliorated the hemorheology and coagulation functions of acute blood stasis(ABS) model rats. Moreover, 27 endogenous metabolites between the CWR group and the ABS group were screened, and the levels were all improved to certain degrees by CWR preadministration. Metabonomics results indicated that ABS was mainly related to linoleic acid metabolism, arachidonic acid metabolism, glycerophospholipid metabolism, sphingolipid metabolism, pentose and glucuronate intercereasonversions, steroid hormone biosynthesis, and primary bile acid biosynthesis. Conclusion: In a word, the metabolomics method is consistent with the holistic view of traditional Chinese medicine(TCM) that can be a powerful means to illustrate the biological activity mechanism of CWR in treating blood stasis and to offer research demonstration for further study on the effector mechanism of TCM.
文摘A high-performance liquid chromatography(HPLC)method has been developed using a CAPCELL PAK ADME(150 mm×4.6 mm,5μm)as analytical column and a gradient elution with 15 min using acetonitrile and 0.1%(in volume fraction)phosphoric acid water(pH=2.2)as the mobile phase.Three active substances in cosmetics were quantitatively detected simultaneously at a detection wavelength of 265 nm.The linear ranges of β-nicotinamide mononucleotides,ergothioneine and nicotinamide are 10~200 mg/L,5~100 mg/L and 5~100 mg/L respectively and the detection limits of three components are 3.0 mg/L,1.5 mg/L and 1.5 mg/L respectively.The recovery rate is 97.1~104.9%,with RSD≤2.0%.The method was applied to quantitative analysis of five samples of cosmetics toner,lotion,cream,essence and gel and three samples of raw materials.The results showed that the results of β-nicotinamide mononucleotide and ergothioneine in five cosmetics were consistent with the product label,while nicotinamide was inconsistent with the label.The purity of the three raw material samples was 99.5%,99.7% and 100.8%respectively.This method offers high precision,accuracy and short analysis time,making it a reliable approach for studying three active ingredients in cosmetics and suitable for quality control of related functional ingredients.
基金the National Natural Science Foundation of China(No.22274021)Natural Science Foundation of Fujian Province(No.2022J01535)for financial support。
文摘Covalent organic frameworks(COFs)have demonstrated great potential in chromatographic separation because of unique structure and superior performance.Herein,single-crystal three-dimensional(3D)COFs with regular morphology,good monodispersity and high specific surface area,were used as a stationary phase for high-performance liquid chromatography(HPLC).The single-crystal 3D COFs packed column not only exhibits high efficiency in separating hydrophobic molecules involving substituted benzenes,halogenated benzenes,halogenated nitrobenzenes,aromatic amines,aromatic hydrocarbons(PAHs)and phthalate esters(PAEs),but also achieves baseline separation of acenaphthene and acenaphthylene with similar physical and chemical properties as well as environmental pollutants,which cannot be quickly separated on commercial C18 column and a polycrystalline 3D COFs packed column.Especially,the column efficiency of 17303-24255 plates/m was obtained for PAEs,and the resolution values for acenaphthene and acenaphthylene,and carbamazepine(CBZ)and carbamazepine-10,11-epoxide(CBZEP)were 1.7and 2.2,respectively.This successful application not only confirmed the great potential of the singlecrystal 3D COFs in HPLC separation of the organic molecules,but also facilitates the application of COFs in separation science.
基金National Natural Science Foundation of China,Grant/Award Number:81973476Chinese Society of Toxicology,Grant/Award Number:CST2021CT101。
文摘Background:Polygonum multiflorum-induced liver injury(PM-DILI)has significantly hindered its clinical application and development.Methods:This study investigates the variation in content and toxicity of dian-thrones,the toxic components of P.multiflorum,during different processing cycles.We employed the ultra-high-performance liquid chromatography triple quadrupole mass spectrometry method to quantify six dianthrones in raw P.multiflorum and formulations processed with a method called nine cycles of steaming and sunning.Additionally,toxicity assessments were conducted using human normal liver cell line L02 and zebrafish embryos.Results:Results indicate a gradual reduction in dianthrones content with increasing processing cycles.Processed formulations exhibited significantly reduced cytotoxic-ity in L02 cells and hepatotoxicity in zebrafish embryos.Conclusions:Our findings elucidate the relationship between processing cycles and P.multiflorum toxicity,providing theoretical support for its safe use.
基金The work was supported by Universiti Kebangsaan Malaysia(UKM),CRIM under Grant GUP-2020-085.
文摘Soil is of particular interest to the forensic community because it can be used as valuable associative evidence to link a suspect to a victim or a crime scene.Liquid chromatography is a powerful analytical tool for organic compound analysis.Recently,high-performance liquid chromatography(HPLC)has proven to be an efficient method for forensic soil analysis,especially in discriminating soils from proximity locations.However,ultra-performance liquid chromatography(UPLC),which is much more sensitive than HPLC,has never been explored in this context.This study proposed a UPLC method for profiling non-volatile organic compounds in three Malaysian soils(red,brown and yellowish-brown soils).The three soils were analysed separately to assess the effects of individual chromatographic parameters:(a)elution programme(isocratic vs.two gradient programmes);(b)flow rate(0.1 vs.0.2 mL/min);(c)extraction solvent(acetonitrile vs.methanol)and(d)detection wavelength(230 vs.254 nm).The injection volume and total run time were set to 5μL and 35 min,respectively.Consequently,each soil sample gave 24 different chromatograms.Results showed that the most desirable chromatographic parameters were(a)isocratic elution;(b)flow rate at 0.2 mL/min and(c)acetonitrile extraction solvent.The proposed UPLC system is expected to be a feasible method for profiling non-volatile organic compounds in soil,and is more chemical-efficient than a comparable HPLC system.
文摘Methods for determining nine low molecular weight organic acids in root exudates were developed by using reversed phase high performance liquid chromatography with UV (ultraviolet) detection at 214 nm. The mobile phase was 18 mmol L -1 kH 2PO 4 adjusted to pH 2.25 with phosphoric acid and the flow rate was 0.3 mL min -1 . The analytical column was a reversed phase silica based C 18 column (Shim pack CLC ODS). The root exudates were collected through submerging the whole root system into aerated deionized water for 2 hours. The filtered exudate solutions were concentrated to dryness by rotary evaporation at 40 °C, dissolved in 10 mL mobile phase. The chromatographic conditions of organic acid determination were analyzed. The results showed that there was a high selectivity and sensitivity in the organic acid determination by reversed phase high performance liquid chromatography. Coefficients of variation for organic acid determination were lower than 10% except lactic acid. The recoveries were consistently between 80.1% to 108.3%. Detection limits were approximately 0.05 to 4.5 mg L -1 for organic acids except succinic acid with the detection limit of 7.0 mg L -1 . Phosphorus deficiency may contribute to the release of organic acids in soybean root exudates especially malic, lactic and citric acids.
基金financially supported in part by the National Natural Science Fund of China for Distinguished Young Scholars(No.81825023)National Natural Science Foundation of China(No.82003979)Natural Science Foundation of Shanghai(No.23ZR1459100)。
文摘Small peptides have attracted increasing attention for their unique features and diverse biological functions.Achieving rapid separation and accurate quantification,however,remains a challenge because of their low abundance and the co-existence of numerous structural isomers.In this study,we developed a novel approach using isotope chemical labeling for ultrasensitive determination of di/tripeptides in biological samples.We successfully synthesized a novel derivatization reagent,4-(2-(ethoxymethylene)-3-oxobutanamido)-N,N,N-trimethylbenzenaminium iodide(EOTMBA)as well as its deuterium-labeled isotope reagent(d_(3)-EOTMBA).A total of 97 small peptides,including 89 dipeptides and 8 tripeptides,could be completely derivatized in methanol within 1.5h at 60℃.After EOTMBA labeling,analysis of these di/tripeptides were achieved within 22 min by LC-MS/MS analysis.The method demonstrated 86.3%-113%accuracy and the limit of quantification ranged from 0.25 fmol/L to 5 nmol/L.Using this method,we achieved ultrasensitive and accurate quantification of di/tripeptides in 147 plasma,49 urine and 46 bile samples obtained from healthy individuals and patients with biliary tract diseases.The identified differential di/tripeptide biomarker panels showed promising diagnostic performance for patients with biliary tract cancer with area under the receiver operating curve values from 0.870 to 0.996.Furthermore,this method was successfully applied to quantify di/tripeptides in the extract of an animal-derived traditional Chinese medicine,Eupolyphaga sinensis Walker.These findings highlight the possible application of the analytical method in clinics and for the purposes of quality control of traditional Chinese medicines.
文摘In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Scientific C18 column (250 mm×4.6 mm, 5 μm) as the chromatographic column and acetonitrile and water as the mobile phase, and the excitation wavelength and emission wavelength of fluorescence detector were 286 and 430 nm, respectively. The response was high, and the linear range was 0.5-10.0 ng/ml. The lowest limit of detection was 0.11 ng/ml, and the average recovery was 92.5%. This method is suitable for quantitative analysis of benzo[a]pyrene content in edible oil.
基金Supported by Youth Talent Project of Education Department Scientific Research Plan of Hubei Province(Q20232904).
文摘Carbendazim belongs to the benzimidazole fungicides,which can be used for control lots of fungi pathogens.High-performance liquid chromatography is frequently used for the analysis of carbendazim in all kinds of samples.In most occasions,the developed methods were applied for the simultaneous detection of a huge number of pesticides.Thus,an analytical method via UPLC-FLD was developed,and the sample preparation process was optimized by studying the effect of extraction solvent,approach,time and purification absorbent on the recovery rate of carbendazim.The results showed the optimized method for analysis was ultrasonication-assisted extraction with acetonitrile for 1 min,and subsequent purification by C18.In this occasion,the established analytical method of carbendazim in tomato samples displayed good linearity,accuracy and precision.
文摘Aim To establish a reversed-phase liquid chromatographic (LC) method forsimultaneous determination of tetramethylpyrazine (TMP) and aspirin in a new compound formulation.Methods Chromatographic separation of the two drugs was achieved on a Diamonsil C_(18) column, usinga binary mixture of methanol-1.5% acetic acid (35:65, V/V, pH = 3.1) as mobile phase at a flow rateof 1.0 mL·min^(-1). Results Separation was completed in less than 12 min. Benzoic acid was used asthe internal standard. Recoveries at levels corresponding to 80 % to 120 % of the label claim ofthe formulation ranged from 99.6 to 100.3 % for aspirin and from 99.9 to 101.3% for TMP. The linearrange was 12.6 - 150.9 μg·mL^(-1)(r= 0.9997, n = 5) for aspirin and 25.0- 300.0 μg·mL^(-1) (r =0.9999, n = 5) for TMP. Conclusion The method developed can be used for the simultaneousdetermination of TMP and aspirin in pharmaceutical preparations.
