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凝胶渗透色谱净化高效液相色谱-串联质谱法检测辛辣蔬菜中咪鲜胺等7种农药残留 被引量:5
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作者 丁葵英 高彦 +3 位作者 于金玲 孙军 赵晗 李凯 《检验检疫学刊》 2013年第5期38-43,共6页
建立了辛辣蔬菜基质中咪鲜胺、异菌脲、虫酰肼、噻螨酮、涕灭威、涕灭威亚砜和涕灭威砜7种农药残留量的凝胶渗透色谱-分散固相萃取技术相结合净化高效液相色谱串联质谱检测法。样品经乙腈提取,氮气吹干,环己烷-乙酸乙酯(1+1)溶液溶解后... 建立了辛辣蔬菜基质中咪鲜胺、异菌脲、虫酰肼、噻螨酮、涕灭威、涕灭威亚砜和涕灭威砜7种农药残留量的凝胶渗透色谱-分散固相萃取技术相结合净化高效液相色谱串联质谱检测法。样品经乙腈提取,氮气吹干,环己烷-乙酸乙酯(1+1)溶液溶解后,凝胶渗透色谱与分散固相萃取法相结合进行净化,反相高效液相色谱柱分离后,采用液相色谱-串联质谱法在分时段多反应监测模式下进行测定,外标法定量。结果表明:7种农药在0.005-2.0μg/mL范围内线性关系均良好(r2在0.995-0.999),且所有农药检出限和定量限均低于国际限量要求;在定量限、5倍和10倍定量限的添加水平下,辛辣蔬菜中7种农药的平均回收率介于60%-120%,相对标准偏差不大于5.0%。该方法定性、定量准确,干扰小,能用于辛辣蔬菜基质中7种农药残留的检测,能很好的满足我国进出口辛辣蔬菜中这7种农药限量的严格要求。 展开更多
关键词 凝胶渗透 液相色谱-串联质谱 多反应监测 农药残留量 辛辣蔬菜基质
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Identification of Pigments from Jujube Fruit Skin 被引量:2
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作者 张琼 沈广宁 +2 位作者 王淑贞 祝恩元 周广芳 《Agricultural Science & Technology》 CAS 2010年第4期110-112,183,共4页
[Objective]The aim was to identify the composition of pigments from Jujube fruit skin.[Method]Pigments were extracted from'Lubei Dongzao','Lajiao Zao','Chengwu Dongzao','Dabailing'and identificated by using hi... [Objective]The aim was to identify the composition of pigments from Jujube fruit skin.[Method]Pigments were extracted from'Lubei Dongzao','Lajiao Zao','Chengwu Dongzao','Dabailing'and identificated by using high performance liquid chromatography-mass spectrometry(HPLC-MS).[Result]The results showed that eight flavanols and four to five flavonols were detected,no anthocyanins was detected.The contents of flavonoids were differnt in four varieties.The contents of flavanols(11 mg/g) and flavonols(1.78 mg/g) in'Dabailing' were one-time higher than other varieties.Quercetin 3 rutinoside was the major flavonol.[Conclusion]The research provided theoretical basis for further study on mechanism of Jujube pigment turnning into the red. 展开更多
关键词 JUJUBE HPLC-MS FLAVANOLS FLAVONOLS Anthocyanins
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Rapid analysis and identification for the alkaloids from Ranunculus japonicus by UPLC /Q-TOF-MS
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作者 钟艳梅 冯毅凡 谭毓治 《Journal of Measurement Science and Instrumentation》 CAS 2014年第3期87-93,共7页
To establish a rapid and effective method for analysis and identification of the alkaloids from Ranunculus japoni- cus Thunb by ultra-performance liquid chromatogaraphy with quadruple-time-of-flight mass spectrometry ... To establish a rapid and effective method for analysis and identification of the alkaloids from Ranunculus japoni- cus Thunb by ultra-performance liquid chromatogaraphy with quadruple-time-of-flight mass spectrometry (UPLC/Q-TOF- MS) and discuss their fragmentation regularity, the UPLC/Q-TOF-MS was used to identify the alkaloids from Ranunculus japonicus Thunb by their MS data, tandem characteristic fragment ions and standards. In the end, 12 alkaloids were identi- fied from Ranunculus japonicus for the first time, and their fragmentation regularity was discussed. Thus, a rapid and effec- tive analysis and identification method for the alkaloids from Ranunculus japonicus by UPLC/Q-TOF-MS is established. 展开更多
关键词 ALKALOIDS ultra-performance liquid chromatogaraphy with quadruple-time-of-flight mass spectrometry (UPLC/Q-TOF-MS) Ranunculus japonicas
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Determination of Sulfadimidine in Royal Jelly by C_(18)-functionalized Magnetic Silica Nanoparticles Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry
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作者 李金峰 李颖 +3 位作者 蒋原 薛峰 戴劲 朱海 《Agricultural Science & Technology》 CAS 2012年第11期2278-2280,共3页
[Objective] This study aimed to develop a method of C_18-functionalized magnetic silica nanoparticles solid phase extraction-high performance liquid chro- matography-tandem mass spectrometry for the determination of s... [Objective] This study aimed to develop a method of C_18-functionalized magnetic silica nanoparticles solid phase extraction-high performance liquid chro- matography-tandem mass spectrometry for the determination of sulfadimidine in royal jelly. [Method] The royal jelly samples were pretreated by MCX SPE column and C_18-functionalized magnetic silica nanoparticles, and the purified samples were de- tected by HPLC-MS/MS. [Result] The detection method showed a good linear rela- tionship in the range of 5-80 ugkg (r=0.993 1). The recovery ranges were between 93%- 104% with the relative standard deviations (RSD) below 11.3%. [Conclusion] Combined with automation equipment, the method is simple, fast, time-saving, and easy to real- ize the automation of sulfadimidine in the royal jelly samples before determination. 展开更多
关键词 Solid phase extraction Magnetic silica nanoparticles Sulfadimidine Highperformance liquid chromatography-tandem mass spectrometry
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A Study on Triacylglycerol Composition and the Structure of High-Oleic Rapeseed Oil 被引量:3
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作者 Mei Guan Hong Chen +4 位作者 Xinghua Xiong Xin Lu Xun Li Fenghong Huang Chunyun Guan 《Engineering》 SCIE EI 2016年第2期258-262,共5页
The composition of fatty acids in triacylglycerides (TAGs) and their position on the glycerol backbone de- termine the nutritional value of vegetable oil. In this study, gas chromatography and high-performance liqui... The composition of fatty acids in triacylglycerides (TAGs) and their position on the glycerol backbone de- termine the nutritional value of vegetable oil. In this study, gas chromatography and high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) were used to analyze the compo- sition and distribution of fatty acids in TAGs of different rapeseed oils. Our results show the content of oleic acid in higb-oleic-acid rapeseed oil to be about 80%. In terms of the number of acyl carbon atoms (CN), TAGs with CN52-54 were most abundant, with a maximum concentration at CN54 (80%). The main type of TAG was oleic-oleic-oleic (OOO), accounting for 71.75%, while oleic-oleic-linoleic (OOL) accounted for ?.56%, oleic-oleic-linolenic (OOLn) accounted for 4.81%, and stearic-oleic-oleic (SO0) accounted for 4.74%. Oleic acid in high-oleic-acid rapeseed oil was distributed in the following order of preference: sn-2 〉 sn-1/3. In high-erucic-acid rapeseed oil, however, oleic acid was enriched at the sn-1/3. These data show that the content of oleic acid can be as high as about 80% in high-oleic-acid material. This finding suggests that high-oleic-acid rapeseed oil has high nutritional value. 展开更多
关键词 Brassica napus Fatty acid Triacylglycerol
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Accumulation and depuration of pectenotoxins in brown crab Cancer pagurus 被引量:1
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作者 李兆新 《Chinese Journal of Oceanology and Limnology》 SCIE CAS CSCD 2009年第2期389-394,共6页
Pectenotoxins (PTXs) are a group of marine algal toxins. In this study, the accumulation and depuration of pectenotoxins in brown crab Cancer pagurus were investigated. Crabs were fed with toxic blue mussels Mytilus e... Pectenotoxins (PTXs) are a group of marine algal toxins. In this study, the accumulation and depuration of pectenotoxins in brown crab Cancer pagurus were investigated. Crabs were fed with toxic blue mussels Mytilus edulis for 21 days and then depurated for 42 days. Toxins were extracted with methanol from the digestive glands of contaminated crabs, uncontaminated crabs (control group) and from blue mussels for comparison. Extracts were analyzed by liquid chromatograph coupled with tandem mass spectrometry (LC-MS-MS). The concentrations of PTX-2, PTX-2 SA, 7-epi-PTX-2 SA, and PTX-12 were analyzed in two batches of toxic blue mussels and the crabs. A one-compartment model was applied to describe the depuration of PTXs. The half-life of PTXs was estimated to be 6–7.5 days. After depuration for 42 days, the amount of PTXs measured in the crab digestive glands was less than 1 μg/kg. 展开更多
关键词 pectenotoxins brown crab blue mussel ACCUMULATION DEPURATION Cancer pagurus Mytilus edulis
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Detection of 36 antibiotics in coastal waters using high performance liquid chromatography-tandem mass spectrometry 被引量:14
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作者 那广水 顾佳 +4 位作者 葛林科 张蓬 王震 刘春阳 张琳 《Chinese Journal of Oceanology and Limnology》 SCIE CAS CSCD 2011年第5期1093-1102,共10页
Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more ... Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more attention to the threat of antibiotics to coastal ecosystems, researchers have often focused on relatively few antibiotics, because of the absence of suitable analytical methods. We have therefore developed a method for the rapid detection of 36 antibiotic residues in coastal waters, including tetracyclines (TCs), sulfanilamides (SAs), and quinolones (QLs). The method consists of solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis, using electrospray ionization (ESI) in positive mode. The SPE was performed with Oasis HLB and Oasis MCX cartridges. Chromatographic separation on a Cr8 column was achieved using a binary eluent containing methanol and water with 0.1% formic acid. Typical recoveries of the analytes ranged from 67.4% to 109.3% at a fortification level of 100 ng/L. The precision of the method, calculated as relative standard deviation (RSD), was below 14.6% for all the compounds. The limits of detection (LODs) varied from 0.45 pg to 7.97 pg. The method was applied to detemaine the target analytes in coastal waters of the Yellow Sea in Liaoning, China. Among the tested antibiotics, 31 were found in coastal 'waters, with their concentrations between the LOD and 212.5 ng/L. These data indicate that this method is valid for analysis of antibiotics in coastal waters. The study first reports such a large number of antibiotics along the Yellow Sea coast of Liaoning, and should facilitate future comprehensive evaluation of antibiotics in coastal ecosystems 展开更多
关键词 ANTIBIOTICS high performance liquid chromatography-tandem mass spectrometry SOLID-PHASEEXTRACTION coastal waters
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Elimination of matrix effects during analysis of perfluorinated acids in solid samples by liquid chromatography tandem mass spectrometry 被引量:2
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作者 李飞 赵志领 +2 位作者 沈春花 曾庆玲 刘淑坡 《Journal of Central South University》 SCIE EI CAS 2012年第10期2886-2894,共9页
Matrix effects can significantly hamper the accuracy and precision of the analysis results of perfluorinated acids (PFAs) in environmental solid samples. Several methods, such as standard addition, isotopically labe... Matrix effects can significantly hamper the accuracy and precision of the analysis results of perfluorinated acids (PFAs) in environmental solid samples. Several methods, such as standard addition, isotopically labeled internal standards, clean-up of SPE (solid phase extraction) eluents by dispersive graphitized carbon sorbent and substitution of eletrospray ionization (ESI) source by atmosphere pressure photoionization (APPI) source, were demonstrated for elimination of matrix effects in quantitative analysis of PFAs in solid samples. The resuRs indicate that matrix effects can be effectively eliminated by standard addition, but instrumental analysis time will be multiplied. Isotopically labeled internal standards can effectively negate matrix effects of PFAs with the same perfluorocarbon chain length, but is not valid for the other analytes. Although APPI can eliminate matrix effects for all analytes, it is only suitable for analysis of high pollution levels samples. Clean-up of SPE eluents by dispersive graphitized carbon sorbent not only effectively negate the impact of matrix effect, but also avoid frequent clean of the ESI in order to maintain instrumental sensitivity. Therefore, the best method for elimination of matrix effects is the usage of dispersive graphitized carbon sorbent for clean-up of SPE elution. 展开更多
关键词 matrix effects perfluorinated acids solid samples hydrophobic organic contaminants
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Determination of Forechlorfenuron Residue in Fruits and Vegetables by QuEChERS Extraction and HPLC-MS/MS
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作者 胡江涛 俞凌云 +2 位作者 帅培强 于刚 何开蓉 《Agricultural Science & Technology》 CAS 2017年第9期1686-1690,共5页
[Objective] A quick extraction method of QuEChERS-HPLC-MS/MS was established to determine forechlorfenuron in fruits and vegetables. [Method] Fruits and vegetables were extracted with 0.1% acetic acid of acetonitrile ... [Objective] A quick extraction method of QuEChERS-HPLC-MS/MS was established to determine forechlorfenuron in fruits and vegetables. [Method] Fruits and vegetables were extracted with 0.1% acetic acid of acetonitrile solution and pu- rified by QuEChERS, and then forechlorfenuron residues were determined by HPLC- MS/MS. [Result] The limits of detection (LODs) and low determination limit (LOQ) for the forechlorfenuron was 1.0 vg/kg and 5.0 pg/kg in fruits and vegetables, re- spectively. Regression equations of these hormones had a good linear relationship (FF〉0.999) within 2.0-100.0 vg/L. The average recoveries of forechlorfenuron was in the range of 72.0-115. 0% with the coefficients of variation between 1.5% and 9.8% at the spiked levels of 10.0-500.0 μg/kg. [Conclusion] The method can be applied for the determination of the forechlorfenuron in fruits and vegetables. 展开更多
关键词 DETERMINATION Forechlorfenuron Fruits and vegetables HPLC-MS/MS
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Rapid Analysis of Nicotine in Mushrooms Using QuEChERS Extraction and Liquid Chromatography Tandem Mass Spectrometry
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作者 A. Santilio R. Dommarco 《Journal of Food Science and Engineering》 2011年第1期27-34,共8页
A procedure based on the QuEChERS methodology and Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) is described, for the determination of Nicotine in mushrooms. QuEChERS methodology was used to determine Ni... A procedure based on the QuEChERS methodology and Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) is described, for the determination of Nicotine in mushrooms. QuEChERS methodology was used to determine Nicotine in dried and fresh mushrooms under basic conditions with primary secondary amino sorbent (PSA) clean up. The chromatography was performed on C 18 reversed phase column using a gradient of acetonitrile and ammonium formiate lmM pH = 3.4 as mobile phase at a flow rate of 0.3 mL min^-1. Nicotine was determined by using Nicotine-d3 as internal standard. Limit of quantification (LOQ) was 0.01 mg kg^-1 for both fresh and dried mushrooms. Calibration curve was linear over the concentration range of 0.01-2.3 mg mL^-1, with r2 〉 0.99. As for recoveries in dried mushrooms, spiking levels of 0.32 mg kg^-1 and 2 mg kg^-1 were considered whereas for the fresh mushrooms the recoveries were determined at 0.036 mg kg^-1 and 0.36 mg kg^-1. Satisfactory results were obtained for both matrices and the recoveries proved to range from 105% to 135%, with a standard deviation in the range 17-20. The method was applied to the analysis of Nicotine to assess the levels of nicotine in fresh and dried mushrooms. 展开更多
关键词 QUECHERS NICOTINE MUSHROOMS PESTICIDES RESIDUES liquid chromatography tandem mass spectrometry (LC/MS/MS)
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Bioequivalence of Two Brands of Valsartan 80 mg Coated Breakable Tablets in 15 Healthy Algerian Volunteers: A Pilot Study
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作者 Mansouri. K.,Behloul. S. Cherait. I., Nekhoul. K. +1 位作者 K., Hadjaz. I. M Mansouri. M. B. 《Journal of Pharmacy and Pharmacology》 2017年第9期661-667,共7页
A randomized, two-way, crossover study was conducted in 15 fasting, healthy, Algerian volunteers to compare the bioavailability of two brands of Valsartan 80 mg coated breakable tablets. The present study aimed to eva... A randomized, two-way, crossover study was conducted in 15 fasting, healthy, Algerian volunteers to compare the bioavailability of two brands of Valsartan 80 mg coated breakable tablets. The present study aimed to evaluate the intra-subject variability of this active substance in the Algerian population. The test brand was compared to TAREG (Novartis) as the reference product. The study was performed at the bioequivalence center of the national control laboratory for pharmaceuticals products, in joint venture with University Hospital Center Ibn Badis, Constantine, Algeria. The drug was administered with 200 mL of water after a 10 h overnight fasting on two treatment days separated by one week washout period. After dosing, serial blood samples were collected for a period of 24 h. A reliable, simple, and robust liquid chromatography-tandem mass spectro-metric (LC-MS/MS) method has been developed and validated that employs protein precipitation (or denaturation) for the estimation of valsartan in human plasma using losartan as internal standard. The assay was found to be linear over the range of 50-5,000 ng/mL, with a lower limit of quantitation of 50ng/mL. Various pharnaacokinetic parameters including AUC0-t, AUC∞, Cmax, Tmax, and TI/2 were determined from plasma concentrations of both formulations and found to be in good agreement with reported values. The pharmacokinetical and statistical analysis was conducted with Kinetica 4.4.1. AUC0.t, AUC0-∞ and Cmax were tested for bioequivalence after log-transformation of data. No significant difference was found based on ANOVA; 90% confidence interval ([85.82%, 118.76%] for AUC0.t [86.09%, 118.83%] for AUC0-∞) of test/reference ratio for these parameters were found within bioequivalence acceptance range of 80-125%. But for the Cmax, the 90% confidence interval of test/reference ratio wasn't in this acceptance range [90.18%, 131.07%] .The results of PK analysis suggested that the reference and test formulations ofvalsartan 80 mg coated breakable tablets weren't bioequivalent during fasting state in these healthy algerian volunteers. 展开更多
关键词 VALSARTAN BIOEQUIVALENCE LC-MS/MS pharmacokinetics.
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Bioequivalence of Two Brands of Metformin 850 mg Coated Tablets in 12 Healthy Algerian Volunteers: A Pilot Study
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作者 Mansouri, K. Aissa, L. +7 位作者 Bounab, A. H., Hadjaz I. M. Nekhoul, K. Djellouli, S. Kheddouci, L. Cherait, I. Behloul, S. Mansouri, M. B. 《Journal of Pharmacy and Pharmacology》 2017年第10期736-741,共6页
A randomized, two-way, crossover study was conducted in 12 fasting, healthy, algerian volunteers to compare the bioavailability of two brands of metformin hydrochloride 850 mg coated tablets. The present study aimed t... A randomized, two-way, crossover study was conducted in 12 fasting, healthy, algerian volunteers to compare the bioavailability of two brands of metformin hydrochloride 850 mg coated tablets. The present study aimed to appreciate the bioequivalence of the generic product and to evaluate the intra-subject variability of this active substance in the Algerian population. The test brand was compared to Glucophage (Merck UK) as the reference product. The study was performed at the bioequivalence center of the national control laboratory for pharmaceuticals products from 03 to 04, 2011, in joint venture with specialized medical hospital center of E1 Hadi Flici, Algiers, Algeria. The drug was administered with 200 mL of water after a 10 h overnight fasting on two treatment days separated by one week washout period. After dosing, serial blood samples were collected for a period of 12 h. A reliable, simple, and robust liquid chromatography-tandem mass spectro-metric (LC-MS/MS) method has been developed and validated for estimation of metformin in human plasma using propranolol as internal standard. The analytes were extracted from plasma by using the protein precipitation extraction technique. The assay was found to be linear over the range of 50-3000 ng/mL with a lower limit of quantitation of 50 ng/mL. Various pharmacokinetic parameters including AUC0-t, AUC0-∞, Cmax, Tmax, and T1/2 were determined from plasma concentrations of both formulations and found to be in good agreement with reported values. The pharmacokinetical and statistical analysis was conducted with Kinetica 4.4.1. AUC0-t, AUC0-∞ and Cmax were tested for bioequivalence after log-transformation of data. No significant difference was found based on ANOVA; 90% confidence interval ([91.62 %, 115.66%] for AUC0-t, [92.07 %, 115.53 %] for AUC0-∞; [94.58%, 119.58 %] for Cmax) of test/reference ratio for these parameters were found within bioequivalence acceptance range of 80-125%. Based on these statistical inferences, it was concluded that Metformin hydrochloride test is bioequivalent to Glucophage. 展开更多
关键词 Metformin hydrochloride BIOEQUIVALENCE LC-MS/MS PHARMACOKINETICS
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Extraction Condition Optimization and Identification of Phenols from Lonicerae flos
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作者 GAO Wei LI Lang +2 位作者 YU Lian-fang DING Hui-juan DING Sheng-hua 《Agricultural Science & Technology》 CAS 2024年第3期21-30,共10页
Polyphenols were obtained from the natural dried Lonicerae flos by ultrasound-assisted extraction with ethanol as the solvent.Single factor experiment and response surface methodology were employed to optimize the ext... Polyphenols were obtained from the natural dried Lonicerae flos by ultrasound-assisted extraction with ethanol as the solvent.Single factor experiment and response surface methodology were employed to optimize the extraction conditions.Ultra-performance liquid chromatrography(UPLC)-tandem mass spectrometry(MS/MS)was employed to identify polyphenols based on the plant widely targeted metabolomics database in a qualitative and quantitative manner.The results showed that the optimal extraction conditions for total phenols from Lonicerae flos were ultrasound-assisted extraction with a solid-to-liquid ratio of 10∶1 g/mL and 57%ethanol at 70 W and 60°C for 11 min.The yield of total phenols extracted under the optimal conditions reached 71.08 mg/g.The phenols in Lonicerae flos were mainly chlorogenic acid isomers,and the flavonoids were mainly nobiletin,galuteolin,and homoarbutin. 展开更多
关键词 Lonicera flos Total phenols Ultra-performance liquid chromatrography(UPLC)-tandem mass spectrometry(MS/MS) Response surface methodology Phenols
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A method for the quantitative determination of glycyrrhetic acid in plasma by LC-MS/MS and its application in a pharmacokinetic study of ammonium glycyrrhetate 被引量:2
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作者 张静 张蕊 +4 位作者 魏春敏 袁桂艳 刘晓燕 王本杰 郭瑞臣 《Journal of Chinese Pharmaceutical Sciences》 CAS 2011年第4期383-389,共7页
A simple and rapid liquid chromatography-tandem mass spectrometry(LC-MS/MS)method was developed and validated for the quantitative determination of glycyrrhetic acid(GA),metabolite of glycyrrhizin and glycyrrhetat... A simple and rapid liquid chromatography-tandem mass spectrometry(LC-MS/MS)method was developed and validated for the quantitative determination of glycyrrhetic acid(GA),metabolite of glycyrrhizin and glycyrrhetate,in human plasma.GA and internal standard(IS,thiamphenicol)were separated on a C_(18)column by elution with acetonitrile-ammonium acetate solution(5 mmol/L)(70:30,v/v)after a simple liquid-liquid extraction with ethyl acetate.The flow rate was 0.8 mL/min. They were detected by tandem mass spectrometry in the negative ion multiple reaction monitoring(MRM)mode with ion transitions of m/z 469.3→355.3 for GA and m/z 354.1→185.0 for IS.The calibration curve was linear over GA concentration range of 0.5-500 ng/mL(r^20.99),with intra-and inter-day precisions(RSD)of less than 7.1%,and mean extraction recovery of 74.3%. The method was used for the pharmacokinetic study of ammonium glycyrrhetate after its oral administration of a single dose of 75 mg ammonium glycyrrhetate tablet in humans.The main pharmacokinetic parameters of GA were as follows:AUC_(0-t) (3457.26±1999.01)ng·h/mL;AUC_(0-∞)(3708.85±2428.36)ng·h/mL;MRT_(0-t)(19.69±4.03)h;MRT_(0-∞)(22.83±8.45)h;t_(1/2)Z (11.71±7.77)h;T_(max)(13.40±4.84)h;CLz/F(29.17±19.82)L/h;Vz/F(487.38±518.07)L;C_(max)(215.85±99.88)ng/mL. 展开更多
关键词 Glycyrrhetic acid PHARMACOKINETICS LC-MS/MS Ammonium glycyrrhetate
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Simultaneous quantification of eighteen constituents in traditional Chinese medicine XiaoShuanTongLuo by UPLCMS/ MS 被引量:2
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作者 赵艳 刘敏 +3 位作者 杨钊 王少华 李杨 杜冠华 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2014年第4期225-232,共8页
XiaoShuanTongLuo (XSTL) is an important multi-herbal formula widely used as a traditional Chinese medicine (TCM). In this paper, an ultra-performance liquid chromatography-electrospray ionization tandem mass spect... XiaoShuanTongLuo (XSTL) is an important multi-herbal formula widely used as a traditional Chinese medicine (TCM). In this paper, an ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometric method (UPLC-ESI-MS/MS) was developed for the simultaneous identification and quantification of 18 chemical constituents in the extract of XSTL. The analysis was performed in multiple-reaction monitoring (MRM) mode using positive and negative electrospray ionization (ESI). A BEH C18 (2.1 mm× 100 mm, 1.7 μm) column with a gradient mobile phase of methanol-0.1% aqueous formic acid solution at a flow rate of 0.2 mL/min was used for separation. The standard curves of most components showed good linearity over the concentration range of 0.001-0.5 μg/mL with r = 0.9896-0.9996. The relative standard deviations (RSD) of intra-day and inter-day precision were all lower than 15% at low, middle, and high concentration levels. The RSD of stability analysis in 24 h were also lower than 15%. The validated method was employed to quantify 18 active components simultaneously in four different commercial brands of XSTL products in various dosage forms. The developed method was rapid, accurate, sensitive, and reproducible for the quality control of XSTL. 展开更多
关键词 Traditional Chinese medicine XiaoShuanTongLuo Ultra-performance liquid chromatography Triple quadrupole tandem mass spectrometer Quality control
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An UPLC-MS/MS application to investigate the chemical composition of the ethanol extract from Anoectochilus chapaensis and its hypoglycemic activity in insulin-resistant HepG2 cells
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作者 蔡金艳 倪俊 赵林 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2016年第5期380-386,共7页
Anoectochilus chapaensis Gagnep. (Orchidaceae) was named as the "king of medicine" because of its excellent efficacy for the treatment of diabetes. However, the bioactive constituents are unknown. An ethanol extra... Anoectochilus chapaensis Gagnep. (Orchidaceae) was named as the "king of medicine" because of its excellent efficacy for the treatment of diabetes. However, the bioactive constituents are unknown. An ethanol extract from A. chapaensis showed significant stimulating effect on glucose consumption in HepG2 cells. The chemical composition was investigated by UPLC-MS/MS in negative electrospray ionization (ESI) mode, and 63 compounds including flavonoids, triterpenoids, and aliphatic acids were tentatively identified by accurate mass and characteristic fragments. Moreover, the method of hypoglycemic screening with insulin resistant HepG2 cells and UPLC-MS/MS might be potentially useful in rapid and efficient characterization and primary prediction of natural products prior to traditional isolation. 展开更多
关键词 UPLC-MS/MS HYPOGLYCEMIC HepG2 cells Anoectochilus chapaensis
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Preparation of the nanostructured lipid carriers of artemisinin and its pharmacokinetic evaluation 被引量:2
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作者 代华灵 高伟祺 +2 位作者 张国顺 王锐利 张淑秋 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2017年第3期180-186,共7页
Artemisinin(ART) is a widely used active drug for malaria, including severe and cerebral malaria. However, its therapeutic efficacy is affected by its lower bioavailability. In the present study, nanostructured lipi... Artemisinin(ART) is a widely used active drug for malaria, including severe and cerebral malaria. However, its therapeutic efficacy is affected by its lower bioavailability. In the present study, nanostructured lipid carriers(NLCs) were proposed as carrier of ART to improve pharmacokinetic properties of the drug. ART-NLC was prepared by high-pressure homogenization based on orthogonal design. The particle size, zeta potential, encapsulation efficiency(EE) and percentage of drug loading(DL) of ART-NLC were(53.06±2.11) nm,(–28.7±3.59) m V, 73.9%±0.5% and 11.23%±0.37%, respectively. ART-NLC showed the sustained release characteristics and scarcely the hemolysis effect on human red blood cells. The pharmacokinetics of ART-NLC for rats after tail intravenous injection(i.v) or intraperitoneal injection(i.p) were investigated by liquid chromatography-tandem mass spectroscopy(LC-MS/MS). And ART solution was designed as control preparation. For rats of i.v groups, the AUC0–∞((707.45±145.65) ng·h/m L) of ART-NLC were significantly bigger than that of ART((368.98±139.58) ng·h/m L). The MRT((3.38±0.46) h) of ART-NLC was longer than that of ART((1.39±0.61) h). And similar results were observed for rats of i.p groups. The AUC0–∞((1233.06±235.57) ng·h/m L) and MRT((4.97±0.69) h) of ART-NLC were both bigger than those of ART, which were(871.17±234.03) ng·h/m L) and(1.75±0.31) h), respectively. Compared with ART, ART-NLC showed a significant increase in AUC0–∞(P〈0.05) and MRT(P〈0.001) for both i.p and tail i.v administrations. 展开更多
关键词 ARTEMISININ Nanostructured lipid carriers PHARMACOKINETICS LC-MS/MS
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A rapid and simple ultraperformance liquid chromatography coupled to tandem mass spectrometry(UPLC-MS/MS) method for the detection of glucuronic acid-conjugated steroid metabolites
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作者 戎怿 黄碧云 +2 位作者 黄珺珺 朱柳 刘夏雯 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2016年第4期291-301,共11页
In the present study, we effectively detected 10 steroids and glucuronic acid-conjugated steroid metabolites in 12 min by ultraperformance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). Ster... In the present study, we effectively detected 10 steroids and glucuronic acid-conjugated steroid metabolites in 12 min by ultraperformance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). Steroids testosterone (T), 5ct-dihydrotestosterone (DHT), androsterone (ADT), etiocholanolone (ETIO), estradiol (E2) and their glucuronide conjugates were well-separated on an Eclipse Plus C18 column (2.1 mm×50 ram, RRHD 1.8μm). The mobile phase consisted of a mixture of methanol and ultrapure water (containing I mM ammonium formate) at a ratio of 60:40 (v/v), and the flow rate was set at 0.25 mL/min. The LC eluate was detected by electrospray ionization (ESI) source in both positive and negative ion modes. Neutral loss (NL of 176, 194, 211 and 229 Da in positive mode) and precursor ion (PI ofm/z 141,159 and 177 in positive mode and 75, 85 and 133 in negative mode) methods were applied for the detection of steroid glucuronides. The multiple reaction monitoring (MRM) transitions were m/z 289.3→97.1,291.3→105, 291.3→199.2, 273.2→145.4 and 255.2→159.1 for T, DHT, ADT, ETIO and E2 in positive mode, respectively; as well as m/z 463.3→85 for T glucuronide (T-G), m/z 465.3→75 for DHT glucuronide (DHT-G), ADT glucuronide (ADT-G), ETIO glucuronide (ETIO-G) and m/z 447.3→271 for E2 glucuronide (Ez-G) in negative mode. In addition, the analytical method was also applied for the detection of steroid glucuronides in pooled human liver microsomes (HLM), which might serve as a basis for further investigation of steroid metabolism in vivo and in vitro. 展开更多
关键词 Steroid glucuronides Ultraperformance liquid chromatography coupled to tandem mass spectrometry Human liver microsome
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Determination of chlorpromazine in porcine muscle using high performance liquid chromatography-tandem mass spectrometry
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作者 张露 黄雯 蒋心惠 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2015年第10期690-694,共5页
A rapid and accurate high performance liquid chromatography tandem mass spectrometry(HPLS-MS) method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitril... A rapid and accurate high performance liquid chromatography tandem mass spectrometry(HPLS-MS) method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitrile to precipitate proteins and followed by extraction with tert--butyl methyl ether(TBME). The separation was performed on a 5 μm Agilent XDB--C18 column with gradient elution. The mobile phase A was 0.01 mol/L ammonium formate in water and mobile phase B was acetonitrile. The flow rate was at 0.8 mL/min. Quantification was performed on a triple-quadrupole tandem mass spectrometer using the multiple selected reaction monitoring(MRM) mode. Transition of m/z +319.1 to 58.1 was used for the quantification of chlorpromazine. The method was validated at the concentration range of 0.4040 μg/kg to 8.080 μg/kg for chlorpromazine with correlation coefficient of 0.9999. The spiked recoveries were more than 80.0% and the limit of detection(LOD) was 0.052 μg/kg. The developed method, which offers advantages of convenience, rapid, specificity and higher sensitivity, can be used for determination of chlorpromazine hydrochloride in porcine muscles. 展开更多
关键词 High performance liquid chromatography-tandem mass spectrometry Chlorpromazine hydrochloride Porcine muscle Residual quantification
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Urinary metabolomics analysis of the anti-depressive effects of Hemerocallis citrina extracts in a simulated microgravity-induced rat model of depression 被引量:4
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作者 Teng Xu Yan Wang +7 位作者 Cong Lu Li Feng Linxi Fan Jing Sun Bei Fan Qiong Wang Xinmin Liu Fengzhong Wang 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2020年第3期176-191,共16页
We investigated the antidepressant-like activity of Hemerocallis citrine Baroni extract(HCE)in a simulated microgravity(SMG)-induced rat model of depression using a metabolomics method.A rat model,generated via 14 d o... We investigated the antidepressant-like activity of Hemerocallis citrine Baroni extract(HCE)in a simulated microgravity(SMG)-induced rat model of depression using a metabolomics method.A rat model,generated via 14 d of SMG induction,was validated from the reduced sucrose preference and the enhanced immobility time in the forced swimming test.HCE and paroxetine reversed certain metabolite profiles.Anti-depressant effects of HCE might involve the regulation of several metabolic pathways,such as phenylalanine,glutamic acid,and tryptophan metabolism and changes in energy metabolism.5-Hydroxytryptophan,hippuric acid,phenylacetylglycine,citric acid,3-hydroxykynurenine,cyclic AMP,and L-DOPA profiles were altered upon HCE and paroxetine administration.Furthermore,glutamic acid was only regulated in the HCE group,while xanthurenic acid and deoxyuridine were reversed in the positive group,suggesting differences in the mechanisms between the positive drugs and HCE in improving glutamic acid metabolism.This study provided a theoretical foundation for the application of HCE in depression therapy. 展开更多
关键词 Hemerocallis citrina Anti-depressive Ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry Ultra-high performance liquid chromatography coupled to triple-quadrupole mass spectrometry Metabolomics
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