LC-MS/MS测定大鼠血浆中虎杖苷浓度

丁雪鹰; 侯晓丽; 孙铭学; 肖凯

doi:10.3969/j.issn.1006-0111.2012.01.012

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LC-MS/MS测定大鼠血浆中虎杖苷浓度

丁雪鹰, 侯晓丽, 孙铭学, 肖凯

文章导航 > 药学实践与服务 > 2012 > 30(1): 45-48

丁雪鹰, 侯晓丽, 孙铭学, 肖凯. LC-MS/MS测定大鼠血浆中虎杖苷浓度[J]. 药学实践与服务, 2012, 30(1): 45-48. doi: 10.3969/j.issn.1006-0111.2012.01.012

引用本文:

丁雪鹰, 侯晓丽, 孙铭学, 肖凯. LC-MS/MS测定大鼠血浆中虎杖苷浓度[J]. 药学实践与服务, 2012, 30(1): 45-48. doi: 10.3969/j.issn.1006-0111.2012.01.012

ZHU Hengmei, LU Guihua, FANG Shuheng, XU Lili. Pain Management with fentanyl transdermal and morphine subcutaneous injection for the patients with advanced liver cancer pain after intervention therapy[J]. Journal of Pharmaceutical Practice and Service, 2017, 35(1): 75-77. doi: 10.3969/j.issn.1006-0111.2017.01.019

Citation:

DING Xue-ying, HOU Xiao-li, SUN Ming-xue, XIAO Kai. Determination of polydatin in rats plasma by LC-MS/MS[J]. Journal of Pharmaceutical Practice and Service, 2012, 30(1): 45-48. doi: 10.3969/j.issn.1006-0111.2012.01.012

LC-MS/MS测定大鼠血浆中虎杖苷浓度

doi: 10.3969/j.issn.1006-0111.2012.01.012

1.
第二军医大学药学院药剂学教研室,上海 200433
2.
第二军医大学海医系毒物药物研究室,上海 200433

基金项目: 上海市科委中药现代化项目(08DZ1971504);国家自然科学基金(20872179,30472141).

Determination of polydatin in rats plasma by LC-MS/MS

1.
Department of Pharmaceutics, School of Pharmacy, Second Military Medical University, Shanghai 200433, China
2.
Laboratory of Toxicology & Pharmacology, Faculty of Naval Medicine, Second Military Medical University, Shanghai 200433, China

摘要: 目的建立测定大鼠血浆中虎杖苷浓度的LC-MS/MS方法。方法采用LC-MS/MS测定大鼠血浆中虎杖苷的浓度,以二苯乙烯苷为内标,血浆样品用乙腈沉淀蛋白,色谱柱为Agilent Zorbax SB-C₁₈ (100 mm×2.1 mm, 3.5 μm),流动相为甲醇-乙腈-0.1%甲酸水溶液(18∶15∶67),流速0.3 ml/min,柱温30 ℃。结果虎杖苷的线性范围为1.0~5 000.0 ng/ml (r=0.998 4),最低定量检测浓度为1.0
- 虎杖苷 /
- LC-MS/MS /
- 血药浓度
Abstract: Objective To establish a LC-MS/MS method for determination of polydatin concentration in rats plasma. Methods The plasma concentration of polydatin was determined by LC-MS/MS. Using stilbene glucoside as internal standard, after precipitation of the plasma proteins with methanol, the analytes were separated on an agilent zorbax SB-C₁₈ reversed-phase column with methanol-acetonitrile- 0.1% formic acid (18 : 15 : 67, v/v) and detected by electrospray ionization (ESI) mass spectrometry in negative multiple reaction monitoring (MRM) mode. The flow rate was 0.3 ml/min. Column temperature was maintained at 30 ℃. Results The calibration curves with good linearity (r=0.998 4 for plasma sample) were obtained in the range of 1.0~5000.0 ng/ml for polydatin. The lower limit of quantification (LLOQ) was 1.0 ng/ml. Recoveries were around 78% for the extraction from rats plasma, and good precision and accuracy were achieved. The intra-day and inter-day RSD were both less than 15.0%. This method was feasible for the evaluation of pharmacokinetic profiles of polydatin in rats. Conclusion This method was simple, selective and sensitive. It's suitable for the pharmacokinetic research of polydatin in rats plasma.
- polydatin /
- LC-MS/MS /
- plasma drug concentration

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LC-MS/MS测定大鼠血浆中虎杖苷浓度

doi: 10.3969/j.issn.1006-0111.2012.01.012

1. 第二军医大学药学院药剂学教研室,上海 200433

2. 第二军医大学海医系毒物药物研究室,上海 200433

基金项目: 上海市科委中药现代化项目(08DZ1971504);国家自然科学基金(20872179,30472141).

收稿日期: 2011-02-10
修回日期: 2011-12-21

关键词:

虎杖苷 /

LC-MS/MS /

血药浓度

摘要: 目的建立测定大鼠血浆中虎杖苷浓度的LC-MS/MS方法。方法采用LC-MS/MS测定大鼠血浆中虎杖苷的浓度,以二苯乙烯苷为内标,血浆样品用乙腈沉淀蛋白,色谱柱为Agilent Zorbax SB-C₁₈ (100 mm×2.1 mm, 3.5 μm),流动相为甲醇-乙腈-0.1%甲酸水溶液(18∶15∶67),流速0.3 ml/min,柱温30 ℃。结果虎杖苷的线性范围为1.0~5 000.0 ng/ml (r=0.998 4),最低定量检测浓度为1.0

English Abstract

Determination of polydatin in rats plasma by LC-MS/MS

1. Department of Pharmaceutics, School of Pharmacy, Second Military Medical University, Shanghai 200433, China

2. Laboratory of Toxicology & Pharmacology, Faculty of Naval Medicine, Second Military Medical University, Shanghai 200433, China

Received Date: 2011-02-10
Rev Recd Date: 2011-12-21

Keywords:

Abstract: Objective To establish a LC-MS/MS method for determination of polydatin concentration in rats plasma. Methods The plasma concentration of polydatin was determined by LC-MS/MS. Using stilbene glucoside as internal standard, after precipitation of the plasma proteins with methanol, the analytes were separated on an agilent zorbax SB-C₁₈ reversed-phase column with methanol-acetonitrile- 0.1% formic acid (18 : 15 : 67, v/v) and detected by electrospray ionization (ESI) mass spectrometry in negative multiple reaction monitoring (MRM) mode. The flow rate was 0.3 ml/min. Column temperature was maintained at 30 ℃. Results The calibration curves with good linearity (r=0.998 4 for plasma sample) were obtained in the range of 1.0~5000.0 ng/ml for polydatin. The lower limit of quantification (LLOQ) was 1.0 ng/ml. Recoveries were around 78% for the extraction from rats plasma, and good precision and accuracy were achieved. The intra-day and inter-day RSD were both less than 15.0%. This method was feasible for the evaluation of pharmacokinetic profiles of polydatin in rats. Conclusion This method was simple, selective and sensitive. It's suitable for the pharmacokinetic research of polydatin in rats plasma.

丁雪鹰, 侯晓丽, 孙铭学, 肖凯. LC-MS/MS测定大鼠血浆中虎杖苷浓度[J]. 药学实践与服务, 2012, 30(1): 45-48. doi: 10.3969/j.issn.1006-0111.2012.01.012

引用本文:

丁雪鹰, 侯晓丽, 孙铭学, 肖凯. LC-MS/MS测定大鼠血浆中虎杖苷浓度[J]. 药学实践与服务, 2012, 30(1): 45-48. doi: 10.3969/j.issn.1006-0111.2012.01.012

Citation: