Simultaneous determination of aristolochic acid I and podophyllotoxin in Longdan Xiegan pills by HPLC-MS/MS

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Author:  Ya-Jing CAO Jia-Xin WEN Jia-Zhe HU Yu-Hong LAI

Affiliation: Guangdong Institute for Drug Control, Guangzhou 510663, China

Keywords: HLPC-MS/MS Longdan Xiegan pills Highly toxic componets Aristolochic acid I Podophyllotoxin

DOI: 10.19960/j.issn.1005-0698.202305006

Reference: Ya-Jing CAO, Jia-Xin WEN, Jia-Zhe HU, Yu-Hong LAI,Simultaneous determination of aristolochic acid I and podophyllotoxin in Longdan Xiegan pills by HPLC-MS/MS[J].Yaowu Liuxingbingxue Zazhi,2023, 32(5): 522-527.DOI: 10.19960/j.issn.1005-0698.202305006.[Article in Chinese]  Copied

Abstract
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Abstract

Objective An HPLC-MS/MS method was established for the simultaneous determination of aristolochic acid I and podophyllotoxin, the highly toxic components in Longdan Xiegan pills, so as to provide the technical basis for the quality control of Longdan Xiegan pills.

Methods The samples were separated on an Agilent InfinityLab Poroshell 120 EC-C18 column (100 mm×2.1 mm, 2.7 μm) with a gradient elution of 0.1% formic acid solution (containing 5 mmol·L^-1 ammonium acetate)-0.1% formic acid acetonitrile as the mobile phase at a column temperature of 35℃, a flow rate of 0.3 mL·min^-1, and the injection volume of 5 μL. Multi-reaction monitoring (MRM) was applied to the determination in positive ion mode of electrospray ion source, and the quantification was conducted by external standard method.

Results Aristolochic acid I and podophyllotoxin showed a good linear relationship in the range of 9.5-94.9 ng·mL^-1 and 10.0-99.7 ng·mL^-1, respectively, and r was greater than 0.9950. The average recovery rates of aristolochic acid I and podophyllotoxin in Big Honeyed pills were 81.89% (RSD=8.55%) and 84.34% (RSD=8.67%); in the Small Honeyed pills were 82.19% (RSD=7.63%) and 96.05% (RSD=6.18%); in the Concentrated pills were 67.99% (RSD=6.70%) and 94.98% (RSD=5.01%); in the Water pills were 75.98% (RSD=11.37%) and 93.88% (RSD=6.01%) (n=18), respectively.

Conclusion The method is simple and accurate, and could be used for the rapid determination of aristolochic acid I and podophyllotoxin, the highly toxic components in Longdan Xiegan pills.

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