A rapid, sensitive and specific ultra-high-performance liquid chromatography tandem mass spectrometry （UPLC-MS） method was developed for the analysis of tetracycline antibiotics, including tetracycline （TC）, oxyte...A rapid, sensitive and specific ultra-high-performance liquid chromatography tandem mass spectrometry （UPLC-MS） method was developed for the analysis of tetracycline antibiotics, including tetracycline （TC）, oxytetracycline （OTC）, chlortetracycline （CTC） and their 4-epimers （4-epiTCs） in agricultural soil fertilized with swine manure. Soil samples were extracted and cleaned-up with 10 mL EDTA-McIlvaine buffer solution （pH 4.0）, then cleaned-up and pre-concentrated using the Oasis MAX cartridge and then eluted with 1 mL solution by mixing formic acid, methanol and water at a ratio of 2：15：83 （v/v/v）. The purified samples were separated by an ACQUITY UPLC BEH C18 column using acetonitrile and water containing 0.1% formic acid mobile phase and detected by a single quadrupole MS. The limits of detection for the soil extraction method （LODsoil） ranged from 0.6-2.5 lag kg-~ with recoveries from 23.3-159.2%. Finally, the method was applied to an agricultural field in an area with intensive pig-fattening farming. Tetracyclines were detected in soil from 2.8 to 42.4 μg kg-1 soil. These results demonstrate that soil from swine farms can become severely contaminated with tetracycline antibiotics and their metabolites.展开更多
Objective:The absorbed prototypes and metabolites of traditional Chinese medicines in vivo are crucial for identifying their biological functions.However,comprehensive profiling of constituents in vivo is difficult ow...Objective:The absorbed prototypes and metabolites of traditional Chinese medicines in vivo are crucial for identifying their biological functions.However,comprehensive profiling of constituents in vivo is difficult owing to endogenous interference and low metabolite abundance.Therefore,a systematic strategy was proposed for screening and profiling exogenous components in biological matrices based on the mass differences between prototypes and the products of their metabolic reactions.Materials and Methods:Two hundred and forty-seven previously reported metabolic reactions were collected from the relevant literature on the Huangqi-Danshen(HD)herb pair,and a metabolic reaction-based mass difference database was created.The preprocessed data from experimental MS1based on ultra-high-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry were automatically calculated mass differences by R programming and matched with the database to screen potential constituents.Finally,the components were annotated across the MS2data.Results:A total of 164 components were annotated in the plasma samples from the rats after oral administration of HD,of which 20 were confirmed using the reference standards.The major metabolic pathways include methylation,dehydration,cysteine S-binding,glucuronidation,sulfation,and multistep reactions.Conclusions:This study revealed the metabolic characteristics and biotransformation regulation of HD and laid the foundation for elucidating its therapeutic effects.The proposed approach provides advantageous resources for evaluating the metabolites in the complex systems.展开更多
An analytical method was established for the determination of 24 food safety risk factors(18 heterocyclic aromatic amines and six mycotoxins)in synthetic meat and synthetic protein samples,and four microcystins in mic...An analytical method was established for the determination of 24 food safety risk factors(18 heterocyclic aromatic amines and six mycotoxins)in synthetic meat and synthetic protein samples,and four microcystins in microalgae samples using ultra-high-performance liquid chromatographyquadrupole/Orbitrap high-resolution mass spectrometry(UPLC-Q/Orbitrap HRMS).The novel synthetic food was extracted using 50%methanol solution and purified with 3 mL of n-hexane saturated with 50%(volume fraction)methanol solution.For the microalgae samples,extraction was performed with 80%(volume fraction)acetonitrile solution and purified using a PRiME HLB solid-phase extraction column.An ACQUITY HSS T3 column(100 mm×2.1 mm,1.8μm)was used for analyte separation,with 5 mmol/L ammonium acetate containing 0.01%(volume fraction)formic acid and methanol selected as the mobile phase.Gradient elution was adopted.Data acquisition was conducted in both positive and negative modes in full-scan data-dependent secondary scan mode(full MS-ddMS2).Matrix-matched standards were employed for quantification in the external standard method.Additionally,mzVault and TraceFinder were used to establish a screening database for 28 food safety risk factors.The results showed that the relative deviation of the exact mass of 28 food safety risk factors was less than 5×10^(-6),with good linearity in the range of 1-100μg/kg,and a correlation coefficient(r^(2))of≥0.9978.The detection limit ranged from 0.5 to 4μg/kg,and the quantification limit ranged from 1 to 10μg/kg.The method recovery ranged from 70.0%to 119.6%with relative standard deviations ranging from 0.4%to 14.6%(n=6).The method is simple,sensitive,accurate,and suitable for rapid screening of 28 food safety risk factors in novel foods.展开更多
To effectively assess the extent of the mycotoxin contamination of grapes,a method was developed to analyze 22 mycotoxins by ultra-high-performance liquid chromatography coupled with quadrupole/orbitrap high-resolutio...To effectively assess the extent of the mycotoxin contamination of grapes,a method was developed to analyze 22 mycotoxins by ultra-high-performance liquid chromatography coupled with quadrupole/orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS).Samples were extracted and purified using the QuEChERS(quick,easy,cheap,effective,rugged,and safe)procedure.The extracts were separated on a BEH Shield C18 column(100 mm×2.1 mm,1.7μm),using methanol and water with 0.1%formic acid solution and 2 mmol/L ammonium acetate as the mobile phases.The quantification was performed according to a matrix-matched external standard method.There was a good linear relationship within the respective mass concentration ranges of 22 mycotoxins;the correlation coefficients were not less than 0.9981.The limit of quantification was 0.3-10.0μg/kg.Mycotoxin recovery ranged from 68.6%to 109.0%,with a relative standard deviation of 1.28%-12.80%.The method is simple,rapid,highly sensitive,and accurate,making it useful for screening grapes for common and emerging mycotoxins.展开更多
Objective: This study aims to elucidate and quantify the composition of Jiangtang Qingre formula(JQF), delineate the absorbed components in the bloodstream, predict the major biologically active components, and identi...Objective: This study aims to elucidate and quantify the composition of Jiangtang Qingre formula(JQF), delineate the absorbed components in the bloodstream, predict the major biologically active components, and identify potential targets for the treatment of diabetes mellitus(DM). Materials and Methods: The chemical composition and metabolites of JQF were elucidated using ultra-high-performance liquid chromatography(UHPLC)-linear ion trap quadrupole-orbitrap high-resolution mass spectrometry(MS). The various components of JQF were concurrently determined using UHPLC-triple–quadrupole MS. Network pharmacological analysis was employed to explore the bioactive components and potential therapeutic targets in DM. Results: A total of 63 compounds were identified and provisionally characterized, with fiavones, organic acids, and alkaloids emerging as the major chemical constituents. A robust analytical method that enables the simultaneous quantification of 24 representative components was successfully developed. The contents of 11 batches of samples were assessed. Ten prototype components were identified in rat plasma. The pathways associated with the efficacy of JQF in DM treatment were linked to signal transduction, endocrine and immune systems, lipid metabolism, and amino acid metabolism. Conclusion: This study systematically and comprehensively characterized the major chemical components and patterns in JQF, laying the groundwork for understanding its pharmacodynamic mechanisms and clinical applications.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
[Objectives]To establish an HPLC method for the quantitative determination of multiple phenolic acid components in Tetracera asiatica medicinal material,providing a basis for establishing its quality standards.[Method...[Objectives]To establish an HPLC method for the quantitative determination of multiple phenolic acid components in Tetracera asiatica medicinal material,providing a basis for establishing its quality standards.[Methods]An Inertsil ODS-C 18 column(250 mm×4.6 mm,5μm)was used.The mobile phase consisted of acetonitrile-0.2% phosphoric acid solution(10:90).The flow rate was 1.0 mL/min.The detection wavelength was 274 nm.The column temperature was 25℃.The injection volume was 10μL.The content of three components,gallic acid,protocatechuic acid,and protocatechualdehyde,was determined in 13 batches of T.asiatica.[Results]Gallic acid showed good linearity within the range of 0.020-6.400μg/mL,protocatechuic acid within 0.201-6.432μg/mL,and protocatechualdehyde within 0.202-6.464μg/mL(r>0.9990).The average recovery rates ranged from 98.61%to 101.17%,with RSD s between 1.21%and 2.69%.[Conclusions]The quantitative determination method established in this study is simple and feasible,and can provide a basis for the quality evaluation of T.asiatica.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
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
Abstract： In the presem study, we simultaneously quantified the levels of monoamine neurotransmitters （MANTs） and their metabolites （levodopa, norepinephrine, epinephrine, dopamine, 5-HT, 3,4-dihydroxyphenylacetic...Abstract： In the presem study, we simultaneously quantified the levels of monoamine neurotransmitters （MANTs） and their metabolites （levodopa, norepinephrine, epinephrine, dopamine, 5-HT, 3,4-dihydroxyphenylacetic acid, homovanillic acid and 5-hydroxyindole-3-acetic acid） in different brain subregions of rats using a newly developed simple, sensitive and selective high-performance liquid chromatography with fluorescence detection （HPLC-FLD） method. In this new HPLC-FLD method, analytes were directly extracted and separated without deriveatization step within 20 min. The FLD wavelength was set at 280 nm and 330 nm for excitation and emission, respectively. The analytes were separated on an Agilent Eclipse Plus Cls column （4.6 mm×150 mm, 5.0 μm） equipped with an Agilent XDB-C18 security guard column （4.6 mm×12.5 mm, 5.0 lam）, and the column temperature was maintained at 35 ℃. The mobile phase for elution was isocratic. The mobile phase consisted of citric acid buffer （50 mmol/L citric acid, 50 mmol/L sodium acetate, 0.5 mmol/L octane sulfonic acid sodium salt, 0.5 mmol/L Na2EDTA and 5 mmol/L triethylamine, pH 3.8） and methanol （90：10, v/v） at a flow rate of 1.0 mL/min. The detection limit （DL） was 0.9-23 nM for all the MANTs and their metabolites with a sample volume of 50 μL. The method was shown to be highly reproducible in terms of peak area （intraday, 0.08%-1.85% RSD, n = 5）. The simultaneous measurement of these MANTs and their metabolites improved our understanding of the neurochemistry in the central nervous system （CNS） in relation to different addictive drugs （methamphetamine, heroin and their mixture） in drug-addicted rat models.展开更多
The crude and processed Paeoniae Radix Alba-Atractylodis Macrocephalae Rhizoma herbal pairs, originated from Bai-zhu-shao-yao-san, are used to treat different diseases clinically. In order to evaluate the crude and pr...The crude and processed Paeoniae Radix Alba-Atractylodis Macrocephalae Rhizoma herbal pairs, originated from Bai-zhu-shao-yao-san, are used to treat different diseases clinically. In order to evaluate the crude and processed Paeoniae Radix-Atractylodis Macrocephalae Rhizoma herbal pairs, a simple, easy, and sensitive high-performance liquid chromatography coupled with diode array detectors was developed for simultaneous determination of nine bioactive components in the herbal pairs. The calibration curve exhibited good linearity（r2≥0.9992）. The LODs and LOQs were ≤7.30 and 11.53 μg/m L, respectively. The intra-, inter-day and repeatability RSD values of the nine compounds were less than 3.86%, 2.71%, and 4.29%, respectively. The RSD stability values were less than 3.64%. The recovery of the method was in the range of 96.70%–102.10%, with RSD values less than 3.52%. The developed method can be applied to the intrinsic quality control of crude and processed Paeoniae Radix-Atractylodis Macrocephalae Rhizoma herbal pairs.展开更多
Due to their biological and physiological importance,flavonoids receive considerable attention in the literature. Nowadays,high performance liquid chromatography（HPLC）is the most widely used analytical method.In thi...Due to their biological and physiological importance,flavonoids receive considerable attention in the literature. Nowadays,high performance liquid chromatography（HPLC）is the most widely used analytical method.In this review,we summarize the principle of the choice of HPLC column and mobile phase,discuss and compare the features of various detections such as UV,fluorescence detection,electrochemical detection,chemilummescence detection,UV-MS etc.Recent developments in HPLC including ultra-LC and miniaturization of LC（micro-LC,capillary-LC,and nano-LC）,are also discussed.展开更多
The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Gi...The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy.展开更多
A sensitive and selective high performance liquid chromatography coupled with electrospray ionization mass spectrometry （LC-MS） was developed for the quantitative determination of ilexgenin A （IA）,a major componen...A sensitive and selective high performance liquid chromatography coupled with electrospray ionization mass spectrometry （LC-MS） was developed for the quantitative determination of ilexgenin A （IA）,a major component in Radix Ilicis Pubescentis,in rat plasma.Chromatographic separation was performed on a C 18 column,with methanol-5 mM ammonium acetate （80：20,v/v） as the mobile phase.Mass spectrometer was set in negative mode with target ions at m/z 501.1→501.1 for IA and m/z 779.4→779.4 for digoxin （internal standard,IS）.Rat plasma was extracted with ethyl acetate after addition of phosphoric solution and the organic layer was evaporated and reconstituted with mobile phase for LC-MS analysis.The proposed method was validated with a linear range of 1.05-525.5 ng/mL for IA with limit of quantitation （LOQ） at 1.05 ng/mL.Intra-and inter-day precision expressed as relative standard deviation （RSD） were less than 10% at LOQ level and overall recovery was over 80%.This validated method was used successfully for the pharmacokinetic study of IA in rats after oral dosing of IA （100 mg/kg） and some main pharmacokinetic parameters of IA in rats were obtained.展开更多
To develop a sensitive high performance liquid chromatography （HPLC） assay for the determination of trans-resveratrol in mouse liver. The whole liver of a mouse was removed from the body, homogenated, and extracted ...To develop a sensitive high performance liquid chromatography （HPLC） assay for the determination of trans-resveratrol in mouse liver. The whole liver of a mouse was removed from the body, homogenated, and extracted by ethyl acetate. The organic layer was isolated and evaporated to dryness, the residue was reconstituted in 0.2 mL mobile phase for centrifugation, and 50 uL of the supernatant was injected into the/-IPLC instrument. The sample was separated on a Shimadzu ODS column （150 mm × 4.6 mm, 5 um） at 35 ℃ and detected by ultraviolet （UV） detector at the wavelength of 305 nm. The mobile phase consisted of methanol and 0.1 mol/L acetic acid （4：6, v/v） with the flow-rote at 1 mL/min. The limit of detection was 3.0 ng/g in liver homogenate with a signal/noise ratio of 3：1. The linear range of the calibration curve was 5.0-120.0 ng/g. The mean recoveries at the concentrations of 6, 10 and 80 ng/g were 102%, 96.0% and 91.5%, respectively. The RSDs for inter- and intra-day assays were less than 5%. Compared with other reported methods, this method was faster and more sensitive. It was also proved to be of good linearity, selectivity, accuracy and precision, and can be efficiently applied to the pharmacoldnetic study of trans-resveratrol in mouse liver.展开更多
The aim of this study was to rapidly isolate the major effective flavanoids from the extract of safflower（Carthamus tinctorius） using ODS medium pressure liquid chromatography（MPLC） and semi-preparative HPLC, guid...The aim of this study was to rapidly isolate the major effective flavanoids from the extract of safflower（Carthamus tinctorius） using ODS medium pressure liquid chromatography（MPLC） and semi-preparative HPLC, guided by a developed fingerprint. Twelve compounds were isolated and their structures were elucidated as kaempferol 3-O-β-D-rutinoside（1）, kaempferol 3-O-β-D-glucoside（2）, rutin（3）, quercetin 3-O-β-D-glucoside（4）, 6-hydroxykaempferol 3,6,7-tri-O-β-D-glucoside（5）, 6-hydroxykaempferol 3-O-β-D-glucoside（6）, 6-hydroxykaempferol 6,7-di-O-β-D-glucoside（7）, 6-hydroxykaempferol 3-O-β-Drutinoside（8）, 6-hydroxykaempferol 3,6-di-O-β-D-glucosyl 7-O-β-D-glucuronide（9）, isosafflomin C（10）, safflomin C（11） and hydroxysafflor yellow A（12） by spectroscopic analysis and comparing with the literature. Our results demonstrated that preparative pressurized liquid chromatography combined with HPLC fingerprint guide is an efficient tool to isolate the target compounds quickly.展开更多
We quantitatively determined four nucleosides, including cytidine, uridine, guanosine, and adenosine, in Carthamus tinctorius L. and Safflower injection. Separation was performed on a Zorbax Eclipse XDB-18 column usin...We quantitatively determined four nucleosides, including cytidine, uridine, guanosine, and adenosine, in Carthamus tinctorius L. and Safflower injection. Separation was performed on a Zorbax Eclipse XDB-18 column using a gradient elution with mobile phases of 0.05% trifluoroacetic acid （TFA） aqueous solution （A） and methanol （B）. The assay was carried out at a flow rate of 1 mL/min at 25 ℃ with detection at 260 nm. Cytidine, uridine, adenosine and guanosine showed good linearity in the ranges of4.02-503μg/mL （r2= 0.9998）, 9.38-1407 μg/mL （rz = 0.9999）, 80.6-8060μg/mL （r2 = 0.9999） and 2.10---630μg/mL （r2 = 0.9987） with average recoveries of 97.2%, 94.5%, 98.6% and 108.6%, respectively. The contents of cytidine, uridine, adenosine and guanosine in different Carthamus tinctorius L. and Safflower injection were significantly different. This is the first report on the quantitative determination of nucleosides in Carthamus tinctorius L. and Safflower injection.展开更多
Aim To quantitatively determine five nucleosides and nucleobases, including cytidine, uridine, guanosine, adenosine and uracil in different parts of Panax notoginseng. Methods Separation was performed on a Zorbax SB-A...Aim To quantitatively determine five nucleosides and nucleobases, including cytidine, uridine, guanosine, adenosine and uracil in different parts of Panax notoginseng. Methods Separation was performed on a Zorbax SB-Aq column using a gradient elution with mobile phase of 8 mmol^L-1 ammonium acetate aqueous solution （A） and methanol （B）. The assay was carried out at a flow rate of 1 mL·min^-1 at 25 ℃ with the diode-array detection at 260 nm. Results Cytidine, uridine, guanosine, adenosine and uracil had good linearity in the ranges of 1.79 - 57.40 μg·mL^-1 （r^2 = 1.0000）, 3.30 - 105.60 μg·mL^-1 （r^2 = 1.0000）, 3.09 - 98.80 μg·mL^ -1（r^2 = 0.9999）, 2.77 - 88.60 μg·mL^-1 （r^2 = 1.0000） and 0.38 - 12.30 μg·mL ^-1 （r^2 = 1.0000） with average recoveries of 93.9%, 96.5%, 92.7%, 93.2% and 98.8%, respectively. The content of cytidine, uridine, guanosine, adenosine and uracil in different parts of P. notogingeng were significantly different. Conclusion This is the first report on quantitative determination of nucleosides and nucleobases in P notoginseng.展开更多
文摘A rapid, sensitive and specific ultra-high-performance liquid chromatography tandem mass spectrometry （UPLC-MS） method was developed for the analysis of tetracycline antibiotics, including tetracycline （TC）, oxytetracycline （OTC）, chlortetracycline （CTC） and their 4-epimers （4-epiTCs） in agricultural soil fertilized with swine manure. Soil samples were extracted and cleaned-up with 10 mL EDTA-McIlvaine buffer solution （pH 4.0）, then cleaned-up and pre-concentrated using the Oasis MAX cartridge and then eluted with 1 mL solution by mixing formic acid, methanol and water at a ratio of 2：15：83 （v/v/v）. The purified samples were separated by an ACQUITY UPLC BEH C18 column using acetonitrile and water containing 0.1% formic acid mobile phase and detected by a single quadrupole MS. The limits of detection for the soil extraction method （LODsoil） ranged from 0.6-2.5 lag kg-~ with recoveries from 23.3-159.2%. Finally, the method was applied to an agricultural field in an area with intensive pig-fattening farming. Tetracyclines were detected in soil from 2.8 to 42.4 μg kg-1 soil. These results demonstrate that soil from swine farms can become severely contaminated with tetracycline antibiotics and their metabolites.
基金supported by the National Natural Science Foundation of China(Grant No.82173963)。
文摘Objective:The absorbed prototypes and metabolites of traditional Chinese medicines in vivo are crucial for identifying their biological functions.However,comprehensive profiling of constituents in vivo is difficult owing to endogenous interference and low metabolite abundance.Therefore,a systematic strategy was proposed for screening and profiling exogenous components in biological matrices based on the mass differences between prototypes and the products of their metabolic reactions.Materials and Methods:Two hundred and forty-seven previously reported metabolic reactions were collected from the relevant literature on the Huangqi-Danshen(HD)herb pair,and a metabolic reaction-based mass difference database was created.The preprocessed data from experimental MS1based on ultra-high-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry were automatically calculated mass differences by R programming and matched with the database to screen potential constituents.Finally,the components were annotated across the MS2data.Results:A total of 164 components were annotated in the plasma samples from the rats after oral administration of HD,of which 20 were confirmed using the reference standards.The major metabolic pathways include methylation,dehydration,cysteine S-binding,glucuronidation,sulfation,and multistep reactions.Conclusions:This study revealed the metabolic characteristics and biotransformation regulation of HD and laid the foundation for elucidating its therapeutic effects.The proposed approach provides advantageous resources for evaluating the metabolites in the complex systems.
基金supported by the National Key Research and Development Program for Young Scientists of China(No.2022YFF1102900).
文摘An analytical method was established for the determination of 24 food safety risk factors(18 heterocyclic aromatic amines and six mycotoxins)in synthetic meat and synthetic protein samples,and four microcystins in microalgae samples using ultra-high-performance liquid chromatographyquadrupole/Orbitrap high-resolution mass spectrometry(UPLC-Q/Orbitrap HRMS).The novel synthetic food was extracted using 50%methanol solution and purified with 3 mL of n-hexane saturated with 50%(volume fraction)methanol solution.For the microalgae samples,extraction was performed with 80%(volume fraction)acetonitrile solution and purified using a PRiME HLB solid-phase extraction column.An ACQUITY HSS T3 column(100 mm×2.1 mm,1.8μm)was used for analyte separation,with 5 mmol/L ammonium acetate containing 0.01%(volume fraction)formic acid and methanol selected as the mobile phase.Gradient elution was adopted.Data acquisition was conducted in both positive and negative modes in full-scan data-dependent secondary scan mode(full MS-ddMS2).Matrix-matched standards were employed for quantification in the external standard method.Additionally,mzVault and TraceFinder were used to establish a screening database for 28 food safety risk factors.The results showed that the relative deviation of the exact mass of 28 food safety risk factors was less than 5×10^(-6),with good linearity in the range of 1-100μg/kg,and a correlation coefficient(r^(2))of≥0.9978.The detection limit ranged from 0.5 to 4μg/kg,and the quantification limit ranged from 1 to 10μg/kg.The method recovery ranged from 70.0%to 119.6%with relative standard deviations ranging from 0.4%to 14.6%(n=6).The method is simple,sensitive,accurate,and suitable for rapid screening of 28 food safety risk factors in novel foods.
基金supported by Science and Technology Program of the State Administration for Market Regulation of China (2020MK014).
文摘To effectively assess the extent of the mycotoxin contamination of grapes,a method was developed to analyze 22 mycotoxins by ultra-high-performance liquid chromatography coupled with quadrupole/orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS).Samples were extracted and purified using the QuEChERS(quick,easy,cheap,effective,rugged,and safe)procedure.The extracts were separated on a BEH Shield C18 column(100 mm×2.1 mm,1.7μm),using methanol and water with 0.1%formic acid solution and 2 mmol/L ammonium acetate as the mobile phases.The quantification was performed according to a matrix-matched external standard method.There was a good linear relationship within the respective mass concentration ranges of 22 mycotoxins;the correlation coefficients were not less than 0.9981.The limit of quantification was 0.3-10.0μg/kg.Mycotoxin recovery ranged from 68.6%to 109.0%,with a relative standard deviation of 1.28%-12.80%.The method is simple,rapid,highly sensitive,and accurate,making it useful for screening grapes for common and emerging mycotoxins.
基金financially by the Scientific and technological innovation project of China Academy of Chinese Medical Sciences (No. CI2021A01606, CI2021A04507, CI2021A04510, Cl2021A04502, CI2021A04509)National Administration of Traditional Chinese Medicine Young Qihuang Scholar Project,ChinaQianjiang Distinguished Expert Project of Hangzhou (2020), China
文摘Objective: This study aims to elucidate and quantify the composition of Jiangtang Qingre formula(JQF), delineate the absorbed components in the bloodstream, predict the major biologically active components, and identify potential targets for the treatment of diabetes mellitus(DM). Materials and Methods: The chemical composition and metabolites of JQF were elucidated using ultra-high-performance liquid chromatography(UHPLC)-linear ion trap quadrupole-orbitrap high-resolution mass spectrometry(MS). The various components of JQF were concurrently determined using UHPLC-triple–quadrupole MS. Network pharmacological analysis was employed to explore the bioactive components and potential therapeutic targets in DM. Results: A total of 63 compounds were identified and provisionally characterized, with fiavones, organic acids, and alkaloids emerging as the major chemical constituents. A robust analytical method that enables the simultaneous quantification of 24 representative components was successfully developed. The contents of 11 batches of samples were assessed. Ten prototype components were identified in rat plasma. The pathways associated with the efficacy of JQF in DM treatment were linked to signal transduction, endocrine and immune systems, lipid metabolism, and amino acid metabolism. Conclusion: This study systematically and comprehensively characterized the major chemical components and patterns in JQF, laying the groundwork for understanding its pharmacodynamic mechanisms and clinical applications.
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Supported by Regional Science Foundation of China,National Natural Science Foundation(No.82160820)General Program of Guizhou Provincial Natural Science Foundation[QianKeHe Foundation-ZK(2023)General153].
文摘[Objectives]To establish an HPLC method for the quantitative determination of multiple phenolic acid components in Tetracera asiatica medicinal material,providing a basis for establishing its quality standards.[Methods]An Inertsil ODS-C 18 column(250 mm×4.6 mm,5μm)was used.The mobile phase consisted of acetonitrile-0.2% phosphoric acid solution(10:90).The flow rate was 1.0 mL/min.The detection wavelength was 274 nm.The column temperature was 25℃.The injection volume was 10μL.The content of three components,gallic acid,protocatechuic acid,and protocatechualdehyde,was determined in 13 batches of T.asiatica.[Results]Gallic acid showed good linearity within the range of 0.020-6.400μg/mL,protocatechuic acid within 0.201-6.432μg/mL,and protocatechualdehyde within 0.202-6.464μg/mL(r>0.9990).The average recovery rates ranged from 98.61%to 101.17%,with RSD s between 1.21%and 2.69%.[Conclusions]The quantitative determination method established in this study is simple and feasible,and can provide a basis for the quality evaluation of T.asiatica.
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.
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.
基金National Natural Science Foundation(Grant No.813 73372)the Open Foundation of State Key Laboratory of Natural and Biomimetic Drugs(Grant No.SKL2012004)Specialized Research Fund for the Doctoral Program of Higher Education of China(Grant No.20110001110021 and 20130001110059)
文摘Abstract： In the presem study, we simultaneously quantified the levels of monoamine neurotransmitters （MANTs） and their metabolites （levodopa, norepinephrine, epinephrine, dopamine, 5-HT, 3,4-dihydroxyphenylacetic acid, homovanillic acid and 5-hydroxyindole-3-acetic acid） in different brain subregions of rats using a newly developed simple, sensitive and selective high-performance liquid chromatography with fluorescence detection （HPLC-FLD） method. In this new HPLC-FLD method, analytes were directly extracted and separated without deriveatization step within 20 min. The FLD wavelength was set at 280 nm and 330 nm for excitation and emission, respectively. The analytes were separated on an Agilent Eclipse Plus Cls column （4.6 mm×150 mm, 5.0 μm） equipped with an Agilent XDB-C18 security guard column （4.6 mm×12.5 mm, 5.0 lam）, and the column temperature was maintained at 35 ℃. The mobile phase for elution was isocratic. The mobile phase consisted of citric acid buffer （50 mmol/L citric acid, 50 mmol/L sodium acetate, 0.5 mmol/L octane sulfonic acid sodium salt, 0.5 mmol/L Na2EDTA and 5 mmol/L triethylamine, pH 3.8） and methanol （90：10, v/v） at a flow rate of 1.0 mL/min. The detection limit （DL） was 0.9-23 nM for all the MANTs and their metabolites with a sample volume of 50 μL. The method was shown to be highly reproducible in terms of peak area （intraday, 0.08%-1.85% RSD, n = 5）. The simultaneous measurement of these MANTs and their metabolites improved our understanding of the neurochemistry in the central nervous system （CNS） in relation to different addictive drugs （methamphetamine, heroin and their mixture） in drug-addicted rat models.
基金The National Natural Science Foundation of China(Grant No.81202918)the Open Project of National First-Class Key Discipline for Science of Chinese Materia Medica,Nanjing University of Chinese Medicine(Grant No.2011ZYX2-006)+2 种基金the Science and Technology Project of Hangzhou,China(Grant No.20130533B68 and 20131813A23)the Chinese Medicine Research Program of Zhejiang Province,China(Grant No.2014ZQ008 and 2015ZQ011)the Science Foundation of Zhejiang Chinese Medical University(Grant No.2011ZY25 and 2013ZZ12)
文摘The crude and processed Paeoniae Radix Alba-Atractylodis Macrocephalae Rhizoma herbal pairs, originated from Bai-zhu-shao-yao-san, are used to treat different diseases clinically. In order to evaluate the crude and processed Paeoniae Radix-Atractylodis Macrocephalae Rhizoma herbal pairs, a simple, easy, and sensitive high-performance liquid chromatography coupled with diode array detectors was developed for simultaneous determination of nine bioactive components in the herbal pairs. The calibration curve exhibited good linearity（r2≥0.9992）. The LODs and LOQs were ≤7.30 and 11.53 μg/m L, respectively. The intra-, inter-day and repeatability RSD values of the nine compounds were less than 3.86%, 2.71%, and 4.29%, respectively. The RSD stability values were less than 3.64%. The recovery of the method was in the range of 96.70%–102.10%, with RSD values less than 3.52%. The developed method can be applied to the intrinsic quality control of crude and processed Paeoniae Radix-Atractylodis Macrocephalae Rhizoma herbal pairs.
基金Administration Bureau of Traditional Chinese Medicine(2007-2008)for Scientific Research Program of TCM (Grant No.HL07057)
文摘Due to their biological and physiological importance,flavonoids receive considerable attention in the literature. Nowadays,high performance liquid chromatography（HPLC）is the most widely used analytical method.In this review,we summarize the principle of the choice of HPLC column and mobile phase,discuss and compare the features of various detections such as UV,fluorescence detection,electrochemical detection,chemilummescence detection,UV-MS etc.Recent developments in HPLC including ultra-LC and miniaturization of LC（micro-LC,capillary-LC,and nano-LC）,are also discussed.
文摘The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy.
文摘A sensitive and selective high performance liquid chromatography coupled with electrospray ionization mass spectrometry （LC-MS） was developed for the quantitative determination of ilexgenin A （IA）,a major component in Radix Ilicis Pubescentis,in rat plasma.Chromatographic separation was performed on a C 18 column,with methanol-5 mM ammonium acetate （80：20,v/v） as the mobile phase.Mass spectrometer was set in negative mode with target ions at m/z 501.1→501.1 for IA and m/z 779.4→779.4 for digoxin （internal standard,IS）.Rat plasma was extracted with ethyl acetate after addition of phosphoric solution and the organic layer was evaporated and reconstituted with mobile phase for LC-MS analysis.The proposed method was validated with a linear range of 1.05-525.5 ng/mL for IA with limit of quantitation （LOQ） at 1.05 ng/mL.Intra-and inter-day precision expressed as relative standard deviation （RSD） were less than 10% at LOQ level and overall recovery was over 80%.This validated method was used successfully for the pharmacokinetic study of IA in rats after oral dosing of IA （100 mg/kg） and some main pharmacokinetic parameters of IA in rats were obtained.
基金Postdoctoral Scientific Research Station of Gansu Yasheng Groups.
文摘To develop a sensitive high performance liquid chromatography （HPLC） assay for the determination of trans-resveratrol in mouse liver. The whole liver of a mouse was removed from the body, homogenated, and extracted by ethyl acetate. The organic layer was isolated and evaporated to dryness, the residue was reconstituted in 0.2 mL mobile phase for centrifugation, and 50 uL of the supernatant was injected into the/-IPLC instrument. The sample was separated on a Shimadzu ODS column （150 mm × 4.6 mm, 5 um） at 35 ℃ and detected by ultraviolet （UV） detector at the wavelength of 305 nm. The mobile phase consisted of methanol and 0.1 mol/L acetic acid （4：6, v/v） with the flow-rote at 1 mL/min. The limit of detection was 3.0 ng/g in liver homogenate with a signal/noise ratio of 3：1. The linear range of the calibration curve was 5.0-120.0 ng/g. The mean recoveries at the concentrations of 6, 10 and 80 ng/g were 102%, 96.0% and 91.5%, respectively. The RSDs for inter- and intra-day assays were less than 5%. Compared with other reported methods, this method was faster and more sensitive. It was also proved to be of good linearity, selectivity, accuracy and precision, and can be efficiently applied to the pharmacoldnetic study of trans-resveratrol in mouse liver.
基金National Science Fund for Excellent Young Scholars(Grant No.81222051)National Key Technology R&D Program"New Drug Innovation"of China(Grant No.2012ZX09103201-036,2012ZX09301002-002-002 and 2012ZX09304-005)
文摘The aim of this study was to rapidly isolate the major effective flavanoids from the extract of safflower（Carthamus tinctorius） using ODS medium pressure liquid chromatography（MPLC） and semi-preparative HPLC, guided by a developed fingerprint. Twelve compounds were isolated and their structures were elucidated as kaempferol 3-O-β-D-rutinoside（1）, kaempferol 3-O-β-D-glucoside（2）, rutin（3）, quercetin 3-O-β-D-glucoside（4）, 6-hydroxykaempferol 3,6,7-tri-O-β-D-glucoside（5）, 6-hydroxykaempferol 3-O-β-D-glucoside（6）, 6-hydroxykaempferol 6,7-di-O-β-D-glucoside（7）, 6-hydroxykaempferol 3-O-β-Drutinoside（8）, 6-hydroxykaempferol 3,6-di-O-β-D-glucosyl 7-O-β-D-glucuronide（9）, isosafflomin C（10）, safflomin C（11） and hydroxysafflor yellow A（12） by spectroscopic analysis and comparing with the literature. Our results demonstrated that preparative pressurized liquid chromatography combined with HPLC fingerprint guide is an efficient tool to isolate the target compounds quickly.
基金Program for Changjiang Scholar and Innovative Team in University(Grant No.985-2-063-112)
文摘We quantitatively determined four nucleosides, including cytidine, uridine, guanosine, and adenosine, in Carthamus tinctorius L. and Safflower injection. Separation was performed on a Zorbax Eclipse XDB-18 column using a gradient elution with mobile phases of 0.05% trifluoroacetic acid （TFA） aqueous solution （A） and methanol （B）. The assay was carried out at a flow rate of 1 mL/min at 25 ℃ with detection at 260 nm. Cytidine, uridine, adenosine and guanosine showed good linearity in the ranges of4.02-503μg/mL （r2= 0.9998）, 9.38-1407 μg/mL （rz = 0.9999）, 80.6-8060μg/mL （r2 = 0.9999） and 2.10---630μg/mL （r2 = 0.9987） with average recoveries of 97.2%, 94.5%, 98.6% and 108.6%, respectively. The contents of cytidine, uridine, adenosine and guanosine in different Carthamus tinctorius L. and Safflower injection were significantly different. This is the first report on the quantitative determination of nucleosides in Carthamus tinctorius L. and Safflower injection.
文摘Aim To quantitatively determine five nucleosides and nucleobases, including cytidine, uridine, guanosine, adenosine and uracil in different parts of Panax notoginseng. Methods Separation was performed on a Zorbax SB-Aq column using a gradient elution with mobile phase of 8 mmol^L-1 ammonium acetate aqueous solution （A） and methanol （B）. The assay was carried out at a flow rate of 1 mL·min^-1 at 25 ℃ with the diode-array detection at 260 nm. Results Cytidine, uridine, guanosine, adenosine and uracil had good linearity in the ranges of 1.79 - 57.40 μg·mL^-1 （r^2 = 1.0000）, 3.30 - 105.60 μg·mL^-1 （r^2 = 1.0000）, 3.09 - 98.80 μg·mL^ -1（r^2 = 0.9999）, 2.77 - 88.60 μg·mL^-1 （r^2 = 1.0000） and 0.38 - 12.30 μg·mL ^-1 （r^2 = 1.0000） with average recoveries of 93.9%, 96.5%, 92.7%, 93.2% and 98.8%, respectively. The content of cytidine, uridine, guanosine, adenosine and uracil in different parts of P. notogingeng were significantly different. Conclusion This is the first report on quantitative determination of nucleosides and nucleobases in P notoginseng.
