scholarly journals Development of a HPLC-MS/MS Method to Determine 11 Bioactive Compounds in Tongmai Yangxin Pill and Application to a Pharmacokinetic Study in Rats

2018 ◽  
Vol 2018 ◽  
pp. 1-11 ◽  
Author(s):  
Jiayuan Shen ◽  
Juan Wei ◽  
Li Li ◽  
Huizi Ouyang ◽  
Yanxu Chang ◽  
...  
Keyword(s):  
Oral Administration ◽  
Gallic Acid ◽  
Bioactive Compounds ◽  
Glycyrrhizic Acid ◽  
Multiple Reaction Monitoring ◽  
Rat Plasma ◽  
Plasma Samples ◽  
Mass System ◽  
Mobile Phases ◽  
Negative Ionization

A sensitive and reliable HPLC-MS/MS method has been developed and validated for simultaneous determination of eleven bioactive compounds (rhein, emodin, stilbene glycoside, liquiritin, ononin, verbascoside, gallic acid, schisandrin, liquiritigenin, glycyrrhizic acid, and isoliquiritigenin) in rat plasma after oral administration of Tongmai Yangxin Pill. The collected plasma samples were prepared by liquid-liquid extraction with ethyl acetate after acidification. Eleven compounds were separated on a CORTECS™ C18 column with mobile phases consisting of 0.1% formic acid in deionized water and acetonitrile. The flow rate was 0.3 mL/min. The detection was performed on a tandem mass system with an electrospray ionization (ESI) source in both positive and negative ionization using multiple-reaction monitoring (MRM) mode. The calibration curves were linear over the range of 8-2000 ng/mL for glycyrrhizic acid; 4-1000 ng/mL for liquiritin; 0.8-200 ng/mL for emodin, gallic acid, ononin, schisandrin, and stilbene glycoside; 0.4-100 ng/mL for isoliquiritigenin, liquiritigenin, rhein, and verbascoside, respectively. The intra- and interday precision of the analytes were less than 9.3% and 8.5%. The intra- and interday accuracy were in the range of -14.0% to 10.3% and -6.5% to 9.6%. Meanwhile, the extraction recovery of the analytes in plasma samples ranged from 85.2% to 109.1% and matrix effect from 89.2% to 113.4%. The developed method was successfully applied to the pharmacokinetics of eleven bioactive compounds in rat plasma after oral administration of Tongmai Yangxin Pill prescription.

scholarly journals A Validated LC-MS/MS Method for Simultaneous Determination of Six Aconitum Alkaloids and Seven Ginsenosides in Rat Plasma and Application to Pharmacokinetics of Shen-Fu Prescription

2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Huizi Ouyang ◽  
Fang Liu ◽  
Zhidan Tang ◽  
Xiaopeng Chen ◽  
Fang Bo ◽  
...  
Keyword(s):  
Oral Administration ◽  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
Reaction Monitoring ◽  
Mass System ◽  
Acid Aqueous Solution ◽  
Interday Precision

A sensitive and reliable LC-MS/MS method has been developed and validated for simultaneous determination of six Aconitum alkaloids (aconitine, hypaconitine, mesaconitine, benzoylaconitine, benzoylhypacoitine, and benzoylmesaconine) and seven ginsenosides (Rb1, Rb2, Rc, Rd, Re, Rf, and Rg1) in rat plasma after oral administration of Shen-Fu prescription. Psoralen was selected as internal standard (IS). Protein precipitation with methanol was used in sample preparation. The chromatographic separation was achieved on a CORTECS™ C18 column with 0.1% formic acid aqueous solution and acetonitrile as mobile phase. The flow rate was 0.3 mL/min. The detection was performed on a tandem mass system with an electrospray ionization (ESI) source in the positive ionization and multiple-reaction monitoring (MRM) mode. The calibration curves of six Aconitum alkaloids and seven ginsenosides were linear over the range of 0.1-50 and 1-500 ng/mL, respectively. The extraction recoveries of the analytes in plasma samples ranged from 64.2 to 94.1%. Meanwhile, the intra- and interday precision of the analytes were less than 14.3%, and the accuracy was in the range of −14.2% to 9.8%. The developed method was successfully applied to the pharmacokinetics of six Aconitum alkaloids and seven ginsenosides in rat plasma after oral administration of Shen-Fu prescription.

scholarly journals Study on Pharmacokinetic and Bioavailability of Tamarixetin after Intravenous and Oral Administration to Rats

2019 ◽  
Vol 2019 ◽  
pp. 1-7
Author(s):  
Jiayuan Shen ◽  
Qi Jia ◽  
Xuhua Huang ◽  
Guangzhe Yao ◽  
Wenjuan Ma ◽  
...  
Keyword(s):  
Oral Administration ◽  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Reaction Monitoring ◽  
Mass System ◽  
Intravenous And Oral Administration ◽  
Interday Precision

In this study, a sensitive and reliable HPLC-MS/MS method was established to quantify tamarixetin in rat plasma. This method was then applied to research on the pharmacokinetic and bioavailability of tamarixetin after intravenous and oral administration in vivo. The study was performed on CORTECS C18 column (4.6 mm × 150 mm, 2.7 μm) using mobile phase composed of methanol-water-formic acid (85 : 15 : 0.1, v/v) at a flow rate of 0.3 mL/min by a tandem mass system with an electrospray ionization (ESI) source in the negative multiple-reaction monitoring (MRM) mode. The calibration curves showed good linearity in the range of 5–4000 ng/mL. The intra- and interday precision of tamarixetin was less than 8.7% and 4.8%, respectively, and accuracy was within ±9.5%. Extraction recovery (91.4–100.0%) and matrix effect (99.4–107.4%) met the guidelines published by regulatory authorities. The oral bioavailability of tamarixetin was 20.3 ± 12.4%.

scholarly journals Simultaneous Quantification of Gallic Acid, Bergenin, Epicatechin, Epicatechin Gallate, Isoquercitrin, and Quercetin-3-Rhamnoside in Rat Plasma by LC-MS/MS Method and Its Application to Pharmacokinetics after Oral Administration of Ardisia japonica Extract

2018 ◽  
Vol 2018 ◽  
pp. 1-9 ◽  
Author(s):  
Xie-an Yu ◽  
John Teye Azietaku ◽  
Jin Li ◽  
Hui Wang ◽  
Fang Zheng ◽  
...  
Keyword(s):  
Oral Administration ◽  
Gallic Acid ◽  
Pharmacokinetic Study ◽  
Rat Plasma ◽  
Epicatechin Gallate ◽  
Chinese Medicinal Herb ◽  
Elution Time ◽  
Internal Standards ◽  
Negative Ionization Mode ◽  
Negative Ionization

Ardisia japonica is a well-known traditional Chinese medicinal herb used as a diuretic, for treating cough and for stopping uterine bleeding. A simple, sensitive, and reliable LC-MS/MS method was developed to determine six active compounds in rat plasma and this method was further applied to the pharmacokinetic study of these compounds after oral administration of Ardisia japonica extract. Acetonitrile was used to precipitate the protein in the plasma samples. Using acetonitrile and formic acid aqueous solution (0.05%) as the mobile phase, the separation of the six compounds and internal standards was achieved at a flow rate of 300 μL min−1 on an Eclipse plus C18 column at an elution time of 16 min. A tandem mass spectrometer having an electrospray ionization (ESI) source was used in the detection of the analytes and internal standards using multiple reactions monitoring (MRM) in the negative ionization mode. The LLOQ was 2, 2, 4, 2, 1, and 0.4 ng mL−1 for gallic acid, bergenin, epicatechin, epicatechin gallate, isoquercitrin, and quercetin-3-rhamnoside, respectively. The validated method was applied to the pharmacokinetic study of gallic acid, bergenin, and quercetin-3-rhamnoside in rat plasma after oral administration of A. japonica extract to rats.

scholarly journals An LC-MS/MS Method for Simultaneous Determination of the Toxic and Active Components of Cortex Periplocae in Rat Plasma and Application to a Pharmacokinetic Study

2019 ◽  
Vol 2019 ◽  
pp. 1-10 ◽  
Author(s):  
Zhen Li ◽  
Yang Li ◽  
Jin Li ◽  
Rui Liu ◽  
Jia Hao ◽  
...  
Keyword(s):  
Oral Administration ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Pharmacokinetic Studies ◽  
Simple Liquid ◽  
Active Components ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass

A sensitive and simple liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to simultaneously determine the toxic and other active components including isovanillin, scopoletin, periplocin, periplogenin, and periplocymarin after oral administration of cortex periplocae extract to rats. Plasma samples were prepared by protein precipitation with methanol. All compounds were separated on a C18 column with gradient elution using acetonitrile and formic acid aqueous solution (0.1%, v/v) as the mobile phase at a flow rate of 0.3 mL/min. The detection of all compounds was accomplished by multiple-reaction monitoring (MRM) in the positive electrospray ionization mode. The LC-MS/MS method exhibited good linearity for five analytes. The lower limit of quantification (LLOQ) was 0.48 ng/mL for scopoletin, periplogenin, and periplocymarin; 2.4 ng/mL for isovanillin and periplocin. The extraction recoveries of all compounds were more than 90% and the RSDs were below 10%. It was found that the absorption of scopoletin and periplocin was rapid in vivo after oral administration of cortex periplocae extract. Furthermore, periplocymarin possessed abundant plasma exposure. The results demonstrated that the validated method was efficiently applied for the pharmacokinetic studies of isovanillin, scopoletin, periplocin, periplogenin, and periplocymarin after oral administration of cortex periplocae extract.

scholarly journals High-throughput cassette assay for drug stability measurement in plasma using direct HPLC-MS/MS

2003 ◽  
Vol 17 (2-3) ◽  
pp. 511-519 ◽  
Author(s):  
Gangfeng Wang ◽  
Yunsheng Hsieh ◽  
K.-C. Cheng ◽  
Kwokei Ng ◽  
Walter A. Korfmacher
Keyword(s):  
High Throughput ◽  
High Performance ◽  
Incubation Temperature ◽  
Drug Stability ◽  
Multiple Reaction Monitoring ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Plasma Samples ◽  
Single Column ◽  
Stability Measurement

A high-throughput semi-automated procedure for simultaneously stability evaluation of multiple compounds in plasma using direct single column high-performance liquid chromatography (HPLC) combined with tandem mass spectrometry (MS/MS) was developed to eliminate the laborious procedures that are traditionally used for stability studies. Untreated human, monkey, mouse and rat plasma samples containing ten drug components were directly injected into a mixed-functional column that provided both protein removal and chromatographic functionality. Ten test compounds were simultaneously assayed using a tandem mass spectrometer in the positive ion mode using multiple reaction monitoring (MRM). Plasma samples containing ten test compounds were placed in a thermostatic autosampler and then sequentially monitored in one analytical procedure. The time between each injection was set about 7 minutes. The peak responses of the test compounds in individual plasma samples were repeatedly determined every 28 minutes. Drug stability in plasma was indicated by the change of the mass chromatographic peak areas for the test compounds and was observed to be a function of animal species, incubation time and incubation temperature. The potential for matrix ionization suppression on the direct single column HPLC-MS/MS system was also investigated using the post-column infusion technique. The proposed cassette assay procedure provides an analytical throughput ten times greater than the single component approach for the evaluation of drug stability in plasma without compromising data quality.

scholarly journals Simultaneous determination and pharmacokinetics studies of five isoflavones in rat plasma by UHPLC-MS/MS after oral administration of Radix Astragali extract

2021 ◽  
Author(s):  
Jianwei Han ◽  
Wenbo Zhu ◽  
Ling Yu ◽  
Yajun Chen ◽  
Gaosong Wu ◽  
...  
Keyword(s):  
Oral Administration ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Radix Astragali ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Mass Spectrometery

AbstractA rapid, sensitive and convenient method based on ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was developed and validated for the simultaneous quantification of calycosin-7-O-β-d-glucoside (CCSG), ononin, calycosin, (6aR,11aR)-9,10-dimethoxypterocarpan-3-O-β-d-glucopyanoside (DPPG), and 7,2′-dihydroxy-3′,4′-dimethoxyisoflavan-7-O-β-d-glucopyanoside (DIFG) in rat plasma after oral administration of the methanol extraction from Radix Astragali. Theophylline played the role of internal standard (IS). Preparation of plasma samples by liquid-liquid extraction method with ethyl acetate after precipitation of protein with methanol. The analytes were detected with a triple quadrupole tandem mass spectrometery (MS) in multiple reaction monitoring (MRM) mode and a positive ion electrospray ionization (ESI). The method was validated with the concentration ranges of 1.96–62.69 ng/mL for CCSG, 1.70–54.5 ng/mL for ononin, 1.85–59.06 ng/mL for calycosin, 2.14–137.24 ng/mL for DPPG and1.96–125.25 ng/mL for DIFG, respectively. The method had the lower limit of quantification (LLOQ) with 0.49, 0.21, 0.92, 1.07, and 0.98 ng/mL for CCSG, ononin, calycosin, DPPG and DIFG respectively, and the precision less than 10%. The RSD of the accuracy was in the range of −4.35–8.91%. The results may be helpful to provide more accurate references to clinical application of this herb.

scholarly journals Comparative Pharmacokinetic Studies of Four Ginsenosides in Rat Plasma by UPLC-MS/MS after Oral Administration of Panax quinquefolius-Acorus gramineus and Panax quinquefolius Extracts

2019 ◽  
Vol 2019 ◽  
pp. 1-13
Author(s):  
Hailong Xie ◽  
Dongxue Wang ◽  
Wenjun Zhang ◽  
Xinjia Yan ◽  
Ying Zhao
Keyword(s):  
Oral Administration ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Critical Role ◽  
Extraction Procedure ◽  
Rat Plasma ◽  
Panax Quinquefolius ◽  
Pharmacokinetic Studies ◽  
Age Related ◽  
Acorus Gramineus

Panax quinquefolius (PQ) and Acorus gramineus (AG) are drug target pairs in traditional Chinese medicine (TCM), which are used to treat age-related diseases. In the present study, we simultaneously determined the contents of four main bioactive ginsenosides (Rb1, Rb2, Rd, and Re) in rat plasma using an ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method. Plasma specimens were purified by using the solid-phase extraction procedure, and separation was performed on Waters ACQUITY UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm) in multiple reaction monitoring (MRM) mode and negative electrospray ionization (ESI) mode. The established UPLC-MS/MS method showed good linear correlation (r ≥ 0.9978), stability (−11.93 to 12.11%), precision (RSD < 14.63%), and recovery (76.43%–95.20%). The lower limit of quantification was 3.6 ng/mL for Rb1, 1.6 ng/mL for Rb2, 1.2 ng/mL for Rd, and 2.5 ng/mL for Re. This validated method was successfully employed to investigate the pharmacokinetics of the four ginsenosides in rat plasma after oral administration of PQ-AG and PQ extracts. The results revealed the pharmacokinetic profiles of PQ-AG drug pair and clarified that AG played a critical role in stimulating the absorption of active ginsenosides in PQ. Collectively, our findings provided valid and reliable evidence for the rational use of PQ-AG in clinical practice.

UPLC-MS/MS determination of chlorogenic acid, hyperoside and astragalin in plasma and its pharmacokinetic application in liver injury rats

2020 ◽  
Vol 16 ◽  
Author(s):  
Ying Zhang ◽  
Shu-ya Xu ◽  
Zhe Jia ◽  
Ting Han ◽  
Meng-nan Liu ◽  
...  
Keyword(s):  
Liver Injury ◽  
Chlorogenic Acid ◽  
Multiple Reaction Monitoring ◽  
Rat Plasma ◽  
Biologically Active ◽  
Hepatoprotective Effect ◽  
Plasma Samples ◽  
Active Components ◽  
Three Components

Background: Cuscutae semen (CS) is reported to show hepatoprotective effect. Chlorogenic acid, hyperoside and astragalin are three major biologically active components from CS. Objective: A sensitive method based on ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed and validated to quantify the three components in rat plasma and was succssfully used to pharmacokinetic study in liver injury rats. Method: Plasma samples were prepared with protein precipitation by acetonitrile. Chromatographic separation was achieved on ACQUITY-XBridge BEH C18 column with a gradient elution using the mobile phase containing 0.05% formic acid in water (A) and acetonitrile (B). The three components were quantified using electrospray ionization (ESI) source in the negative multiple reaction monitoring (MRM) mode. Results and Discussion: Calibration curves of each analyte showed a good linearity with correlation coefficients over 0.99. Accuracies (RE%) and precisions (RSD%) were within 15%. The method was stable. Recovery of the target compounds in plasma samples ranged from 87.00% to 102.29%. No matrix effect was found to influence the quantitative method. Conclusion: The UPLC-MS/MS method was met the acceptance criteria and successfully applied to simultaneous determination of chlorogenic acid, hyperoside and astragalin in rat plasma for the first time. It is suitable for pharmacokinetic application in liver injury rats. It provides the foundation for the further development and utilization for the hepatoprotective effect of cuscutae semen.

scholarly journals Simultaneous Determination and Pharmacokinetics Study of Six Triterpenes in Rat Plasma by UHPLC-MS/MS after Oral Administration of Sanguisorba officinalis L. Extract

Molecules ◽  
2018 ◽  
Vol 23 (11) ◽  
pp. 2980 ◽  
Author(s):  
Chengcui Wu ◽  
Meicun Yao ◽  
Wa Li ◽  
Binbin Cui ◽  
Hongrui Dong ◽  
...  
Keyword(s):  
Oral Administration ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Current Method ◽  
Rat Plasma ◽  
Ion Source ◽  
Pharmacokinetics Study ◽  
Liquid Chromatography Tandem Mass ◽  
Sanguisorba Officinalis

A selective and sensitive ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for the determination of ziyuglycoside I (I), 3β,19α-dihydroxyurs-12-en-28-oic-acid 28-β-d-glucopyranosyl ester (II), 3β-[(α-l-arabinopyranosyl) oxy]-urs-12,18(19)-dien-28-oic acid β-d-glucopyranosyl ester (III), rosamultin (IV), 1β-hydroxyeuscaphic acid (V) and alpinoside (VI) in rats after oral administration of Sanguisorba officinalis L. (S. officinalis) extract. The 3β,19α-dihydroxyurs-12-en-28-oic-acid 28-β-d-glucopyranosyl ester, 3β-[(α-l-arabinopyranosyl) oxy]-urs-12,18(19)-dien-28-oic acid β-d-glucopyranosyl ester, rosamultin, 1β-hydroxyeuscaphic acid and alpinoside in rat plasma were the first report in the pharmacokinetics study in the present study. The analytes were quantified using the multiple reaction monitoring (MRM) mode with the electrospray ion source in positive electrospray ionization. Plasma was extracted with ethyl acetate via liquid–liquid extraction. Bifendate was used as internal standard (IS). The current method was validated for linearity, intra-day and inter-day precisions, accuracy, extraction recovery, matrix effect and stability. The lower limits of quantification of ziyuglycoside I, 3β,19α-dihydroxyurs-12-en-28-oic-acid 28-β-d-glucopyranosyl ester, 3β-[(α-l-arabinopyranosyl) oxy]-urs-12,18(19)-dien-28-oic acid β-d-glucopyranosyl ester, rosamultin, 1β-hydroxyeuscaphic acid and alpinoside were 6.1, 4.9, 1.3, 3.8, 1.5 and 5.7 ng/mL, respectively. Intra-day and inter-day precision and the accuracy of the assay were in range from −9.48 to 12.74%. The extraction recoveries of analytes and bifendate (IS) from rat plasma ranged from 77.17% to 92.48%. Six compounds could be rapidly absorbed into blood (Tmax, 0.58–1.58 h), and then eliminated relatively slowly (t1/2, 6.86–11.63 h). The pharmacokinetic results might contribute to further guide the clinical application of S. officinalis.

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