Ingredient Analysis

Analysis of aristolochic acid Ⅰ and aristolactam Ⅰ in Chitong Xiaoyanling granules by liquid chromatography-mass spectrometry

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  • National Institutes for Food and Drug Control, Beijing 100050, China

Received date: 2021-04-20

  Online published: 2024-06-24

Abstract

Objective: To establish the analysis method of aristolochic acid Ⅰ and aristolactam Ⅰ in Chitong Xiaoyanling granules by liquid chromatography-mass spectrometry (LC-MS). Methods: An Agilent SB-C18 (2.1 mm× 50 mm,1.8 μm) column was used with gradient elution of acetonitrile-0.1% formic acid at a flow rate of 0.3 mL·min-1. The multiple-reaction monitoring mode was used and the detection ion pairs for aristolochic acid Ⅰ were m/z 359.0→ 298.1 (quantitation), m/z 359.0 → 296.1 (qualitation) for aristolochic acid Ⅰ, and m/z 294.0 → 278.9 (quantitation), m/z 294.0 → 251.1 (qualitation) for aristolactam Ⅰ . As a result, the LC-MS method was established to detect the aristolochic acid Ⅰ and aristolactam Ⅰ in Chitong Xiaoyanling granules. And the method was further validated and used to test all samples. Results: The developed method showed good linearity in the range of 51.849-1 036.984 pg and 1.842-36.848 pg with R2≥0.999 5 for aristolochic acid Ⅰ and aristolactam Ⅰ, respectively. The limits of quantification (LOQs) were 26.91 and 0.69 pg, and the average recovery rates were 107.2%-107.4% (RSD 0.5%-2.1%), 98.9%-105.5% (RSD 1.3%-2.9%), respectively. Aristolochic acid Ⅰ was not detected in all the 16 batches of samples. And the conetens of aristolactam Ⅰ were in the range of 0.063-0.763 μg·g-1. Conclusion: The established method is accurate, sensitive and reliable. It can be applied for analysis of aristolochic acid analogues in Chitong Xiaoyanling granules. And it can provide sound scientific basis for the study of safety related components.

Cite this article

LIU Jing, LIU Yang, WU Ying-xue, DAI Zhong, MA Shuang-cheng . Analysis of aristolochic acid Ⅰ and aristolactam Ⅰ in Chitong Xiaoyanling granules by liquid chromatography-mass spectrometry[J]. Chinese Journal of Pharmaceutical Analysis, 2022 , 42(2) : 237 -242 . DOI: 10.16155/j.0254-1793.2022.02.07

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