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A New Method for Simultaneous Determination of Nicotinamide Mononucleotide, Ergothioneine, and Nicotinamide in Cosmetics by Reverse Phase High Performance Liquid Chromatography
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作者 Liu Xin Wu Jianming 《China Detergent & Cosmetics》 2025年第3期98-105,共8页
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
关键词 COSMETICS β-nicotinamide mononucleotide ERGOTHIONEINE NICOTINAMIDE high performance liquid chromatography(hplc)
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Determination of Organic Acids in Root Exudates by High Performance Liquid Chromatography:Ⅱ.Influence of Several Testing Conditions 被引量:2
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作者 SHENJIANBO ZHANGFUSUO 《Pedosphere》 SCIE CAS CSCD 1999年第1期45-52,共8页
Effects of column temperature and flow rate on separation of organic acids were studied by determining nine low-molecular-weight organic acids on reversed- phase C18 column, using high performance liquid chromatograph... Effects of column temperature and flow rate on separation of organic acids were studied by determining nine low-molecular-weight organic acids on reversed- phase C18 column, using high performance liquid chromatography (HPLC) with a wavelength of UV (ultraviolet) 214 urn and a mobile phase of 18 mmol L-1 KH2PO4 buffer solution (pH 2.1). The thermal stability of organic acids was determined by comparing the recoveries of organic acids in different temperature treatments. The relationships between column temperature, flow rate or solvent pH and retention time were analyzed. At low solvent pH, separation efficiency of organic acids was increased by raising the flow rate of the solvent because of lowering the retention time of organic acids. High column temperature was unfavorable for the separation of organic acids. The separating effect can be enhanced through reducing column temperature in organic acid determination due to increasing retention time. High thermal stability of organic acids with low concentrations was observed at temperature of 40 ℃-45℃. Sensitivity and separation effect of organic acid determination by HPLC were clearly improved by a combination of raising flow rate and lowering column temperature at low solvent pH. 展开更多
关键词 chromatographic conditions high performance liquid chromatography (hplc) organic acids root exudates
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On-line enrichment and determination of polycyclic aromatic hydrocarbons in atmospheric particulates using high performance liquid chromatography with fluorescence as detector 被引量:1
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作者 HASHI Yuki WANG Tian-ran +1 位作者 LI Yue-qi LIN Jin-ming 《Journal of Environmental Sciences》 SCIE EI CAS CSCD 2007年第10期1261-1265,共5页
Seven polycyclic aromatic hydrocarbons (PAHs) in atmospheric particulates were determinated by high performance liquid chromatography (HPLC) with fluorescence detector using direction injection and an on-line enri... Seven polycyclic aromatic hydrocarbons (PAHs) in atmospheric particulates were determinated by high performance liquid chromatography (HPLC) with fluorescence detector using direction injection and an on-line enrichment trap column. The method simplified the sample pretreatment, saved time and increased the efficiency. With the on-line trap column, PAHs were separated availably even underground injecting 1.0 ml sample with relatively high column efficiency. The recoveries of the seven PAHs were from 85% to 120% for spiked atmospheric particulate sample. The limit of detection was 15.3-39.6 ng/L (S/N=3.3). There were good linear correlations between the peak areas and concentrations of the seven kinds of PAHs in the range of 1-50 ng/ml with the correlation coefficients over 0.9970. Furthermore, it also indicated that the method is available to determine PAHs in atmospheric particulates well. 展开更多
关键词 on-line enrichment on-line trap column high performance liquid chromatography hplc atmospheric particulate polycyclic aromatic hydrocarbons (PAHs)
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Separation and identification of moxifloxacin impurities in drug substance by high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform ion cyclotron resonance mass spectrometry 被引量:8
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作者 Cai Sheng Wu Zhi Xin Jia +2 位作者 Bao Ming Ning Jin Lan Zhang Song Wu 《Chinese Chemical Letters》 SCIE CAS CSCD 2012年第10期1185-1188,共4页
In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry (HPLC-UV/FrICRMS) method was described for the investigation... In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry (HPLC-UV/FrICRMS) method was described for the investigation of impurity profile in moxifloxacin (MOX) drug substance and chemical reference substance. Ten impurities were detected by HPLC-UV, while eight impurities were identified by using the high accurate molecular mass combined with multiple-stage mass spectrometric data and fragmentation rules. In addition, to our knowledge, five impurities were founded for the first time in MOX drug substance. 展开更多
关键词 Moxifloxacin (MOX) Impurity profile high-performance liquid chromatography coupled with ultraviolet detection and Fouriertransform-ion cyclotron resonance mass spectrometry hplc-UV/bTICRMS)
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Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography coupled with diode array detector and evaporative light scattering detector 被引量:4
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作者 Yi-Kai Shi Fang Cui +3 位作者 Fang-Di Hu Ying-Yan Bi Yu-Feng Ma Shi-Lan Feng 《Journal of Pharmaceutical Analysis》 SCIE CAS 2011年第1期20-25,共6页
A simple and accurate high-performance liquid chromatography(HPLC)coupled with diode array detector(DAD)and evaporative light scattering detector(ELSD)was established for the determination of six bioactive compo... A simple and accurate high-performance liquid chromatography(HPLC)coupled with diode array detector(DAD)and evaporative light scattering detector(ELSD)was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation(ZFP).The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis(HCA),which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation. 展开更多
关键词 high-performance liquid chromatographyhplc diode array detector(DAD) evaporative light scattering detector(ELSD) Zhenqi Fuzheng preparation quantification hierarchical cluster analysis
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Biological Fingerprinting Analysis of Interaction Between Taxoids in Taxus and Microtubule Protein by Microdialysis Coupled with High-performance Liquid Chromatography/Mass Spectrometry for Screening Antimicrotubule Agents 被引量:1
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作者 LEI Xiao-yuan KONG Liang +2 位作者 SU Xing-ye GUO Ming ZOU Han-fa 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2008年第4期411-419,共9页
Some natural products, such as traditional Chinese medicines(TCMs), contain compounds with anticancer activity and have attracted a great interest in recent years as alternative anticancer therapies. A quick and con... Some natural products, such as traditional Chinese medicines(TCMs), contain compounds with anticancer activity and have attracted a great interest in recent years as alternative anticancer therapies. A quick and convenient assay for screening antimicrotubule compounds in which in vitro microdialysis/high-performance liquid chromatography (HPLC) is used to monitor the binding of the compounds extracted from TCM Taxus cuspidata Siebold & Zucc(Taxus) to microtubules is reported. It was observed that the extract of Taxus contains at least five compounds which have affinity interaction with microtubules by biological fingerprinting analysis, and they were identified as the taxoids of taxol, baccatin III, 10-deacetylbaccatin Ⅲ(10-DAB), cephalomannine and 7-epi-10-deacetyltaxol (7-epi-10-DAT) based on the comparison of their high-performance liquid chromatographic/mass spectrometric and UV spectra with those of the standard samples, both assembly-promoting and disassembly-inhibiting characteristics of those compounds were evaluated. It was observed that baccatin Ⅲ and 10-DAB bound to microtubules and the binding degrees were influenced by GTP. Competitive binding behavior of taxol with other four taxoids to microtubules was also investigated. 展开更多
关键词 Microdialysis/high-performance liquid chromatographyhplc Biological fingerprinting analysis TAXOIDS MICROTUBULE TAXUS
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A Sensitive Reversed-Phase High-Performance Liquid Chromatography Method for the Quantitative Determination of Milk Xanthine Oxidase Activity 被引量:1
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作者 Zhongqin Li Ruizhang Guan Hongwei Liu 《Open Journal of Medicinal Chemistry》 2013年第1期26-30,共5页
A new reversed-phase high performance liquid chromatography method was developed to quantitate the activity of xanthine oxidase involved in milk fat globule membrane with xanthine as the substrate and the separation o... A new reversed-phase high performance liquid chromatography method was developed to quantitate the activity of xanthine oxidase involved in milk fat globule membrane with xanthine as the substrate and the separation of product (uric acid). The increment of uric acid in the reaction system was used to calculate the total activity of XO. The optimized assay conditions, linearity of detection, recovery of uric acid and chromatogram were developed in text, indicating this method is simple, rapid and efficient. It is an alternative potential method for the determination of the activity of XO in milk. 展开更多
关键词 XANTHINE OXIDASE (XO) Enzyme Activity Assay REVERSED-PHASE high performance Liquid chromatography (RP-hplc)
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Study on the Flow Injection Micro-Column Pre-Separation System Coupled With High Performance Liquid Chromatography for the Determination of Ecdysterone in Traditional Chinese Medicine
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作者 SHUAI Qin QIN Yong-chao +2 位作者 JIANG Zu-cheng LI Feng LIAO Zhen-huan (College of Chemistry and Environmental Science, Wuhan University, Wuhan 430072, China) 《Wuhan University Journal of Natural Sciences》 CAS 2000年第1期83-88,共6页
A flow injection (FI) micro-column system coupled with high performance liquid chromatography (HPLC) was proposed for the pre-separation and determination of active organic component (ecdysterone) in traditional Chine... A flow injection (FI) micro-column system coupled with high performance liquid chromatography (HPLC) was proposed for the pre-separation and determination of active organic component (ecdysterone) in traditional Chinese medicine, Loulu. The factors influencing separation performance were investigated and optimized. Under the optimal conditions, the contents of ecdysterone in Loulu were determined by HPLC system using MeOH-H_2O (40: 60,V/V) as the mobile phase at a flow rate of 1. 0 mL/min. The calibration curve was linear in the range of 0. 5~ 100 mg/L of ecdysterone concentrations. The detection limit of the analyte was 0. 11mol/L(3) with a precision of 0. 38% RSD (n=7 f c= 10. 0 mg/L). The average recovery of the method was 98. 7%. The proposed method has been applied to determine ecdysterone in practical samples, and the determined values by both external standard method and standard addition method were in good agreement. Compared to the traditional solid extraction method, the system proposed has the advantages of simple procedure, good reproducibility, minimum volume requirement, reduction of matrix interference and low contamination risk. 展开更多
关键词 high performance liquid chromatography(hplc) Flow injection analysis (FIA) ECDYSTERONE traditional Chinese medicine
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Determination of Naringin Content in Rhizoma Drynariae by High Performance Liquid Chromatography
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作者 Huili GONG Guoxia DUAN +4 位作者 Lijun LIU Ruilong XIE Shuo TANG Cuizhi LI Zhiyong LU 《Asian Agricultural Research》 2022年第10期23-25,共3页
[Objectives]To accurately determine the naringin content in Rhizoma Drynariae.[Methods]The high performance liquid chromatography(HPLC)method was applied in the determination of the naringin content in Rhizoma Drynari... [Objectives]To accurately determine the naringin content in Rhizoma Drynariae.[Methods]The high performance liquid chromatography(HPLC)method was applied in the determination of the naringin content in Rhizoma Drynariae.The sample was sonicated at room temperature.The mobile phase was 0.1%phosphoric acid-acetonitrile(75∶25),detected by diode array detector at the wavelength of 284 nm,and quantified by external standard method.[Results]The linearity of naringin was good in the concentration range of 5-500μg/mL with a correlation coefficient of 0.9999.[Conclusions]This method has good linearity,easy operation,correctness and reproducibility as required,and is expected to provide a method for the determination of naringin content in Rhizoma Drynariae. 展开更多
关键词 high performance LIQUID chromatography (hplc) Rhizoma Drynariae NARINGIN
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Simultaneous Determination of Content of VK_(1) and VK_(2) in Milk and Dairy Products by High Performance Liquid Chromatography
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作者 Huili GONG Guoxia DUAN +3 位作者 Lijun LIU Shuo TANG Cuizhi LI Zhiyong LU 《Asian Agricultural Research》 2022年第7期63-68,71,共7页
[Objectives]To make simultaneous determination of vitamin K_(1)(VK_(1))and vitamin K_(2)(VK_(2),mainly MK-4,MK-7 and MK-9)in milk and dairy products.[Methods]A high performance liquid chromatographic method was develo... [Objectives]To make simultaneous determination of vitamin K_(1)(VK_(1))and vitamin K_(2)(VK_(2),mainly MK-4,MK-7 and MK-9)in milk and dairy products.[Methods]A high performance liquid chromatographic method was developed for the simultaneous determination of vitamin K_(1)(VK_(1))and vitamin K_(2)(VK_(2),mainly MK-4,MK-7 and MK-9)in milk and dairy products.After enzymatic digestion,the samples were extracted with hexane for VK_(1),MK-4,MK-7 and MK-9,subjected to gradient elution at excitation wavelength 243 nm and emission wavelength 430 nm,detected by high performance liquid chromatography with fluorescence detector and quantified by external standard method.[Results]The linearity of VK_(1),MK-4,MK-7 and MK-9 was good in the concentration range of 2.5-1000 ng/mL with the correlation coefficients greater than 0.999;The relative standard deviations(RSD)of VK_(1),MK-4,MK-7 and MK-9 in milk powder,liquid milk and yogurt were 1.32%-5.05%,1.10%-2.48% and 2.20%-3.47%,respectively;the recovery rates of VK_(1),MK-4,MK-7 and MK-9 at different levels in milk powder,liquid milk and yogurt were 81.1%-108%,81.8%-103%and 82.1%-99.2%,respectively.[Conclusions]The method is rapid,accurate,reproducible and capable of simultaneous determination of VK_(1),MK-4,MK-7 and MK-9. 展开更多
关键词 high performance liquid chromatography(hplc) Vitamin K_(1) Vitamin K_(2) MK-4 MK-7 MK-9
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Determination of seven active components in Salvia miltiorrhiza herb by matrix solid phase dispersion combined with ion liquid extraction followed by high performance liquid chromatography
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作者 Bo Hong Yanping Wang +1 位作者 Yinglong Han Wenjing Li 《Asian Journal of Traditional Medicines》 CAS 2021年第2期83-97,共15页
A low cost,rapid and sensitive preparation method of silica gel supported ionic liquid(SGSIL)combined with matrix solid phase dispersion(MSPD)followed by high performance liquid chromatography(HPLC)with ultraviolet de... A low cost,rapid and sensitive preparation method of silica gel supported ionic liquid(SGSIL)combined with matrix solid phase dispersion(MSPD)followed by high performance liquid chromatography(HPLC)with ultraviolet detection(UV)is proposed,and it was applied to determine the seven active compounds in Salvia Miltiorrhiza herb.SGSIL and ionic liquid[BMIM]BF4 were used as the adsorbent and the green elution reagent in the MSPD procedure.Several extraction conditions including type of filler and elution solvent,the volume of elution solvent,material liquid ratio were optimized.Under the optimum conditions,the SGSIL-MSPD-HPLC method showed a low limit of detection(LOD,S/N=3)of 0.0122-0.8788μg/mL for standard solution,limit of quantification(LOQ,S/N=10)of 0.0406-2.9292μg/mL for standard solution,wide linear range from 1.56 to 2000μg/mL for all compounds for standard solution,correlation coefficients(r)of more than 0.9990,acceptable reproducibility(relative standard deviations,RSDs<3.54%),and precision of RSDs<3.36%for intra-day,RSDs<3.50%for inter-day.The satisfactory recoveries ranged from 96.4 to 102.5,with RSDs less than 3.45%.The developed SGSIL-MSPD method is easier and more suitable for the determination of the seven active compounds in Salvia Miltiorrhiza herb than the traditional ultrasonic extraction.It was an effective and efficient method for the extraction and quantification of the seven active compounds in traditional Chinese herbal samples. 展开更多
关键词 high performance liquid chromatography(hplc) silica gel supported ionic liquid(SGSIL) matrix solid phase dispersion(MSPD) Salvia miltiorrhiza(SM) DETERMINATION
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HPLC-DAD法测定益气养血口服液中5-羟甲基糠醛
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作者 马彧 王丹彧 +2 位作者 马晓静 宋瑩 崔业波 《质量安全与检验检测》 2026年第1期34-37,共4页
本研究建立了益气养血口服液中5-羟甲基糠醛(5-HMF)的检测方法。采用HPLC-DAD法,Caprisil C_(18)-IP为色谱柱(250 mm×4.6 mm,5μm);流动相为甲醇-0.05%磷酸,梯度洗脱;体积流量为1.0 mL/min;柱温25℃;检测波长284 nm。结果显示,5-... 本研究建立了益气养血口服液中5-羟甲基糠醛(5-HMF)的检测方法。采用HPLC-DAD法,Caprisil C_(18)-IP为色谱柱(250 mm×4.6 mm,5μm);流动相为甲醇-0.05%磷酸,梯度洗脱;体积流量为1.0 mL/min;柱温25℃;检测波长284 nm。结果显示,5-羟甲基糠醛在2.539~55.389μg/mL内线性关系良好(r=1.0000),平均加样回收率为97.0%,RSD为0.2%。不同企业生产的样品中均检出5-羟甲基糠醛。5-羟甲基糠醛的产生可能与益气养血口服液生产工艺相关,建议在益气养血口服液的标准中增加5-羟甲基糠醛检查项。本研究建立的方法简便、准确,可为企业质量控制提供参考。 展开更多
关键词 5-羟甲基糠醛 益气养血口服液 高效液相色谱法
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HPLC测定米氮平透皮软膏含量及其稳定性初步分析
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作者 刘博 郎丰亭 +2 位作者 赵莉 崔亮亮 郝智慧 《中国兽医杂志》 北大核心 2026年第1期64-70,共7页
为了建立检测米氮平透皮软膏中米氮平含量的高效液相色谱(HPLC)方法,并初步分析米氮平透皮软膏的稳定性,本试验使用InertSustain C_(18)色谱柱,以甲醇∶四氢呋喃∶乙腈∶四甲基氢氧化铵缓冲溶液(12.5∶7.5∶15∶65,v/v/v/v)为流动相,检... 为了建立检测米氮平透皮软膏中米氮平含量的高效液相色谱(HPLC)方法,并初步分析米氮平透皮软膏的稳定性,本试验使用InertSustain C_(18)色谱柱,以甲醇∶四氢呋喃∶乙腈∶四甲基氢氧化铵缓冲溶液(12.5∶7.5∶15∶65,v/v/v/v)为流动相,检测波长290 nm,流速1.5 mL/min,柱温40℃对米氮平含量进行测定;并通过光照、高温和高湿稳定性试验以及铝质药用软膏管包装后的加速和长期稳定性试验检测米氮平透皮软膏的稳定性。结果显示,空白溶剂和辅料对米氮平检测无影响,米氮平对照品以50%乙腈为溶剂,进样浓度介于236.78~355.17μg/mL,样品浓度与峰面积的线性关系良好(R^(2)=0.9997)。米氮平平均回收率为100.05%,相对标准偏差(RSD)为0.61%,供试品和对照品溶液在室温放置24 h稳定性良好;稳定性试验中高温(60℃)会使软膏中米氮平含量由100.40%下降至97.26%,而高湿、光照、加速试验和长期试验对软膏中米氮平的含量无影响。结果表明,本试验建立的HPLC方法专属性强、准确度高,可用于米氮平透皮软膏中米氮平含量测定,并且米氮平透皮软膏可采用铝质药用软膏管进行包装,同时应避免高温储藏和运输。 展开更多
关键词 米氮平透皮软膏 高效液相色谱(hplc) 稳定性 质量控制
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HPLC-MS/MS法测定血液肿瘤患者血浆中维奈克拉、伏立康唑和泊沙康唑的浓度及药动学研究
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作者 王浩然 邢晗 +1 位作者 王培乐 杨晶 《中国医院用药评价与分析》 2026年第1期43-47,共5页
目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)法,测定血液肿瘤患者血浆中维奈克拉、伏立康唑和泊沙康唑的浓度,并进行维奈克拉联合伏立康唑或泊沙康唑的药动学研究。方法:选用Shim-pack VP-ODS/C8/Phenyl色谱柱(150 mm×2.0 mm,4.6... 目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)法,测定血液肿瘤患者血浆中维奈克拉、伏立康唑和泊沙康唑的浓度,并进行维奈克拉联合伏立康唑或泊沙康唑的药动学研究。方法:选用Shim-pack VP-ODS/C8/Phenyl色谱柱(150 mm×2.0 mm,4.6μm),以0.1%甲酸甲醇-0.1%甲酸水为流动相,在正离子模式下,对维奈克拉、伏立康唑和泊沙康唑进行检测。选取2022年9月至2023年5月郑州大学第一附属医院收治的同时服用维奈克拉和伏立康唑或泊沙康唑的患者33例,在多次服药后采集血样进行药物浓度检测。结果:维奈克拉、伏立康唑和泊沙康唑分别在血药浓度0.05~10、0.05~10和0.025~5μg/mL范围内线性良好(R^(2)>0.99)。联合应用伏立康唑或泊沙康唑后,维奈克拉的主要药动学参数如下,24 h药时曲线下面积分别为(55.92±25.66)、(81.30±55.64)(μg·h)/mL,表观清除率分别为(2.16±0.98)、(1.61±1.10)L/h。结论:该方法简便、灵敏、准确,可用于血液肿瘤患者血浆中维奈克拉、伏立康唑和泊沙康唑浓度的检测。 展开更多
关键词 高效液相色谱-串联质谱 维奈克拉 伏立康唑 泊沙康唑 药动学
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HPLC法同时测定清瘟解毒口服液中10种有效成分的含量
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作者 任鑫 李静静 +7 位作者 刘双慧 赵伟娟 韩爱霞 邢思毅 宋庆庆 于敏 李元晓 李秋 《中国兽药杂志》 2026年第1期9-14,共6页
为完善清瘟解毒口服液的质量控制方法,利用高效液相色谱法对清瘟解毒口服液中有效成分尿苷、梓醇、腺苷、鸟苷、R,S-告依春、哈巴苷、栀子苷、连翘苷、黄芩苷、哈巴俄苷测定进行研究。用Agilent Polaris C18-A(5μm 250mm×4.6mm)... 为完善清瘟解毒口服液的质量控制方法,利用高效液相色谱法对清瘟解毒口服液中有效成分尿苷、梓醇、腺苷、鸟苷、R,S-告依春、哈巴苷、栀子苷、连翘苷、黄芩苷、哈巴俄苷测定进行研究。用Agilent Polaris C18-A(5μm 250mm×4.6mm)为色谱柱,流动相为0.01%磷酸溶液(A)和甲醇(B),梯度洗脱(0-20min,99% A→88% A;20~65min,88% A→20% A;65~70min A→99%):检测波长(0-30min,210nm;30-65min,245nm)流速为0.8mL/min;柱温30℃;进样量为10μL。结果为峰面积与含量呈良好线性关系。该方法简单准确度高,可用于清瘟解毒口服液中有效成分的含量测定,为控制其产品质量提供依据。 展开更多
关键词 高效液相色谱法 清瘟解毒口服液 黄芩苷 栀子苷
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基于HPLC-DAD-CAD的恒制咳喘胶囊质量均一性分析 被引量:1
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作者 马倩 刘安 +5 位作者 许青霞 郭丛 章军 王茂青 寇晓娣 刘艳 《中国实验方剂学杂志》 北大核心 2025年第3期168-174,共7页
目的:建立15批次恒制咳喘胶囊的指纹图谱,对其中10种指标性成分进行定量分析,并评价恒制咳喘胶囊不同批次产品的质量均一性。方法:采用高效液相色谱-二级管阵列检测器-电喷雾检测器联用法(HPLC-DAD-CAD)建立恒制咳喘胶囊指纹图谱及含量... 目的:建立15批次恒制咳喘胶囊的指纹图谱,对其中10种指标性成分进行定量分析,并评价恒制咳喘胶囊不同批次产品的质量均一性。方法:采用高效液相色谱-二级管阵列检测器-电喷雾检测器联用法(HPLC-DAD-CAD)建立恒制咳喘胶囊指纹图谱及含量测定方法;选择腺苷、鸟苷、香草酸、羟基红花色素A、沉香四醇、柚皮苷、橙皮苷、1,4-二[4(-葡萄糖氧)苄基]-2-异丁基苹果酸酯、人参皂苷Rb1、甘草酸共10种成分作为质量属性指标,对来自2022—2024年共15批(每批3盒)45份恒制咳喘胶囊样品进行定性和定量分析;以批内均一性差异参数(PA)和批间均一性差异参数(PB)表征厂家质量均一性水平;采用聚类热分析表征不同年份样品质量属性指标的同质性和差异性。结果:建立了恒制咳喘胶囊HPLC指纹图谱及定量方法,经方法学考证,方法稳定可靠,可用于该制剂的定性、定量分析;15批样品的指纹图谱相似度0.887~0.975,共标定共有峰13个,指定10个共有峰,均为质量属性指标成分。定量分析结果显示,样品中的腺苷、鸟苷、香草酸、羟基红花色素A、沉香四醇、柚皮苷、橙皮苷、1,4-二[4-(葡萄糖氧)苄基]-2-异丁基苹果酸酯、人参皂苷Rb1、甘草酸的质量分数分别为0.038~0.078、0.115~0.251、0.007~0.018、0.291~0.673、0.122~0.257、0.887~1.905、1.841~3.364、1.412~2.450、2.207~3.112、0.650~1.161 mg·g^(-1),其中人参皂苷Rb1、甘草酸均符合2020年版《中华人民共和国药典》对该制剂的限度要求;15个批次10种指标成分的PA均<10%,表明批内均一性良好,PB为33.86%~92.97%,表明批间均一性较差;聚类热分析显示,不同年份的样品各聚为一类,其中腺苷、鸟苷、羟基红花色素A、柚皮苷、橙皮苷、沉香四醇等6种成分是主要差异性成分。结论:恒制咳喘胶囊的年内质量均一性较好,年间质量均一性不足,可能与法半夏、红花、佛手、陈皮、沉香、香橼等药味的质量差异有关。该研究建立了恒制咳喘胶囊的指纹图谱和多指标含量测定方法,可用于更准确、高效的质量控制和标准提升。 展开更多
关键词 恒制咳喘胶囊 高效液相色谱法(hplc) 二极管阵列检测器(DAD) 电喷雾检测器(CAD) 质量均一性 指纹图谱
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基于HPLC-MS/MS的2种乙酰氨基阿维菌素注射剂在兔体内的药代动力学对比研究 被引量:1
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作者 张贺超 张振东 +4 位作者 刘希望 杨亚军 李世宏 秦哲 李剑勇 《中国畜牧兽医》 北大核心 2025年第5期2295-2304,共10页
【目的】建立兔血浆中乙酰氨基阿维菌素(EPR)的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法,比较2种EPR注射剂在商品兔体内的药代动力学,为后续制剂开发提供支持。【方法】将12只健康新西兰商品兔,雌雄各半,分为参比制剂(市售EPR注射剂... 【目的】建立兔血浆中乙酰氨基阿维菌素(EPR)的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法,比较2种EPR注射剂在商品兔体内的药代动力学,为后续制剂开发提供支持。【方法】将12只健康新西兰商品兔,雌雄各半,分为参比制剂(市售EPR注射剂)组和受试制剂(自研EPR缓释注射剂)组,皮下注射相同剂量的2种制剂,于不同时间点采集血液样本,以莫西菌素为内标,采用HPLC-MS/MS法检测EPR的浓度,并对所建立的方法进行特异性、检测限和定量限、标准曲线、准确度和精密度、基质效应、稳定性考察,以软件Phoenix WinNonlin对实际的采样时间-血药浓度数据进行权重为1/Y的非房室分析,求得2种制剂在兔体内的药代动力学参数。【结果】建立的HPLC-MS/MS分析方法检测限和定量限分别为0.5和1 ng/mL;标准曲线在1~200 ng/mL范围内线性关系良好,且相关系数(R^(2))>0.99;高、中、低及定量限4个浓度的批内和批间准确度在93.70%~107.73%范围内,批内和批间相对标准差(RSD)均<15%。参比制剂和受试制剂中EPR达峰时间(T_(max))分别为(0.39±0.09)和(0.22±0.04)d;峰浓度(C_(max))分别为(112.82±29.40)和(30.86±5.11)ng/mL;半衰期(t_(1/2))分别为(7.14±0.58)和(22.15±1.22)d;药时曲线下面积(AUC_(0→∞))分别为(420.55±21.74)和(300.65±13.62)ng·d/mL;平均滞留时间(MRT)分别为(3.74±0.80)和(41.62±9.04)d。【结论】本研究建立的HPLC-MS/MS分析方法灵敏度和准确度高,稳定可靠,可用于兔血浆中EPR的检测。2种制剂在吸收速率、吸收程度及消除速率方面具有明显差异,与参比制剂相比,受试制剂能显著延长商品兔血浆中EPR存在的时间。 展开更多
关键词 乙酰氨基阿维菌素 高效液相色谱-串联质谱(hplc-MS/MS) 药代动力学 缓释注射剂
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毛发、尿液中依托咪酯及代谢物HPLC-MS/MS检测 被引量:5
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作者 吴永富 王燕军 +3 位作者 代勇 张鑫 周奎霖 蔡玉刚 《刑事技术》 2025年第1期61-67,共7页
本文建立高效液相色谱-三重四极杆串联质谱仪(HPLC-MS/MS)检测毛发和尿液中依托咪酯及其代谢物依托咪酯酸的检测方法。毛发样品经研磨粉碎后,经甲醇超声提取,尿液样品经乙腈沉淀蛋白高速离心过0.22μm滤膜后,采用Agilent Eclipse Plus C... 本文建立高效液相色谱-三重四极杆串联质谱仪(HPLC-MS/MS)检测毛发和尿液中依托咪酯及其代谢物依托咪酯酸的检测方法。毛发样品经研磨粉碎后,经甲醇超声提取,尿液样品经乙腈沉淀蛋白高速离心过0.22μm滤膜后,采用Agilent Eclipse Plus C18 RRHD(3.0 mm×150 mm×1.8μm)色谱柱,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,流速0.5 mL/min;选择电喷雾离子源,多反应监测(MRM)正离子模式进行监测。实验表明,尿液中依托咪酯和依托咪酯酸在0.5~50 ng/mL的浓度范围,毛发中依托咪酯和依托咪酯酸在0.025~2.5 ng/mg浓度范围内线性关系良好,R^(2)值均大于0.9925,提取回收率为91.0%~107.5%,日内和日间精密度RSD为0.4%~7.4%,日内和日间准确度为91.5%~110.8%。对实际案例中的6份毛发和4份尿液样本进行检测,检测结果表明,6份毛发均检出依托咪酯原体,其中2份毛发检出代谢物依托咪酯酸且含量远低于原体;4份尿液中2份检出依托咪酯和代谢物依托咪酯酸且代谢物含量远高于原体。本文建立的方法能快速对吸食依托咪酯人员的毛发和尿液中依托咪酯及代谢物进行定性定量分析。 展开更多
关键词 依托咪酯 依托咪酯酸 高效液相色谱-三重四级杆串联质谱仪(hplc-MS/MS) 毛发 尿液
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基于HPLC-Q-Exactive-MS技术分析蒙药小秦艽花化学成分、体内血清及肺组织移行成分 被引量:1
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作者 王宁 王敏杰 +4 位作者 李君 包福顺 张文雪 郭琪 伊乐泰 《中国民族医药杂志》 2025年第5期29-36,共8页
目的:基于高效液相色谱-四级杆/静电场轨道阱高分辨质谱(HPLC-Q-Exactive-MS)表征蒙药小秦艽花粗提物固有成分、血清移行成分及肺组织移行成分,为阐明其物质基础提供基础。方法:甲醇提取药物,采用色谱柱Agilent ZORBAX SB-Aq(4.6 mm... 目的:基于高效液相色谱-四级杆/静电场轨道阱高分辨质谱(HPLC-Q-Exactive-MS)表征蒙药小秦艽花粗提物固有成分、血清移行成分及肺组织移行成分,为阐明其物质基础提供基础。方法:甲醇提取药物,采用色谱柱Agilent ZORBAX SB-Aq(4.6 mm×150 mm,5μm),流动相甲醇(A)-0.1%甲酸水(B),流速0.35 mL/min,柱温35℃,进样量10μL,质谱采用正、负离子扫描,扫描范围m/z 110~1200;大鼠给予600 mg/mL小秦艽花粗提物连续7日,末次给药后0.5 h、1 h、1.5 h、2 h取血清与肺组织。结果:结合质谱数据和文献信息,在小秦艽花粗提物中鉴别出50个化学成分,包括16个黄酮类成分、11个有机酸类成分、4个环烯醚萜类成分、4个没食子酸酯成分、4个脂肪酸成分、3个氨基酸成分、2个酚酸类成分、2个倍半萜类成分、1个氢醌类成分、1个三萜类成分、1个生物碱类成分、1个鞣质类成分;入药血清鉴别出26个化学成分,包括9个黄酮类成分、9个有机酸类成分、2个酚酸类成分、2个没食子酸酯成分、1个倍半萜类成分、1个环烯醚萜类成分、1个氢醌类成分、1个鞣质类成分、1个三萜类成分;入肺成分中鉴别出17个化学成分,包括个黄酮类8成分、5个有机酸类成分、1个酚酸类成分、1个氢醌类成分、1个鞣质类成分、1个三萜类成分。结论:HPLC-Q-Exactive-MS方法能快速鉴别蒙药小秦艽花的化学成分,为蒙药小秦艽花的药效物质研究奠定基础。 展开更多
关键词 小秦艽花 血清移行成分 肺组织移行成分 高效液相色谱-四级杆/静电场轨道阱高分辨质谱 定性分析 化学成分
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Comparison of the performance of chiral stationary phase for separation of fluoxetine enantiomers
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作者 ZHOU Jie ZHOU Jie +2 位作者 YANG Yi-wen WEI Feng WU Ping-dong 《Journal of Zhejiang University-Science B(Biomedicine & Biotechnology)》 SCIE CAS CSCD 2007年第1期56-59,共4页
Separation of fluoxetine enantiomers on five chiral stationary phases (chiralcel OD-H, chiralcel OJ-H, chiralpak AD-H, cyclobond 1 2000 DM and kromasil CHI-TBB) was investigated. The optimal mobile phase composition... Separation of fluoxetine enantiomers on five chiral stationary phases (chiralcel OD-H, chiralcel OJ-H, chiralpak AD-H, cyclobond 1 2000 DM and kromasil CHI-TBB) was investigated. The optimal mobile phase compositions of fluoxetine separation on each column were hexane/isopropanol/diethyl amine (98/2/0.2, v/v/v), hexane/isopropanol/diethyl amine (99/1/0. l, v/v/v), hexane/isopropanol/diethyl amine (98/2/0.2, v/v/v), methanol/0.2% triethylamine acetic acid (TEAA) (25/75, v/v; pH 3.8) and hexane/isopropanol/diethyl amine (98/2/0.2, v/v/v), respectively. Experimental results demonstrated that baseline separation (Rs〉1.5) of fluoxetine enantiomers was obtained on chiralcel OD-H, chiralpak AD-H, and cyclobond I 2000 DM while the best separation was obtained on the last one. The eluate orders of fluoxetine enantiomers on the columns were determined. The first eluate by chiralcel OJ-H and kromasil CHI-TBB is the S-enantiomer, while by chiralpak AD-H and cyclobond 12000 DM is the R-enantiomer. 展开更多
关键词 FLUOXETINE Chiral stationary phase Enantiomeric separation high performance liquid chromatography hplc
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