| 引用本文: | 马临科,王娟娟,郑成.HPLC-MS/MS测定鱼腥草和复方鱼腥草合剂中马兜铃酸类化合物含量[J].中国现代应用药学,2022,39(15):2011-2015. |
| MA Linke,WANG Juanjuan,ZHENG Cheng.Content Determination of Aristolochic Acid Analogs in Houttuynia Cordata and Compound Yuxincao Mixture by HPLC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2022,39(15):2011-2015. |
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| 摘要: |
| 目的 建立HPLC-MS/MS同时测定鱼腥草药材和复方鱼腥草合剂中马兜铃酸Ⅰ、马兜铃酸Ⅱ和马兜铃内酰胺Ⅰ含量的方法。方法 采用Phenomenex Kinetex C18色谱柱（100 mm×2.1 mm，2.6 μm）；流动相为乙腈和0.2%甲酸水溶液，梯度洗脱，流速为0.3 mL·min–1，柱温为30℃；采用电喷雾离子源，以多反应离子监测模式进行质谱检测。结果 马兜铃酸Ⅰ、马兜铃酸Ⅱ和马兜铃内酰胺Ⅰ分别在11.91~1 985 ng·mL–1（r=0.995 3）、16.87~2 812 ng·mL–1（r=0.995 7）和3.404~567.4 ng·mL–1（r=0.996 6）内有良好的线性关系。各化合物平均回收率为85%~111%，RSD为0.2%~6.7%。马兜铃酸Ⅰ检测限为2.395 ng·mL–1、定量限为7.984 ng·mL–1；马兜铃酸Ⅱ检测限为3.389 ng·mL–1，定量限为10.50 ng·mL–1；马兜铃内酰胺Ⅰ检测限为0.334 2 ng·mL–1，定量限为1.113 ng·mL–1。结论 该方法专属性好，灵敏度高，准确可靠耐用，可以用于鱼腥草合剂中马兜铃酸Ⅰ、马兜铃酸Ⅱ和马兜铃内酰胺Ⅰ的含量测定。 |
| 关键词: 鱼腥草 复方鱼腥草合剂 马兜铃酸 HPLC-MS/MS |
| DOI：10.13748/j.cnki.issn1007-7693.2022.15.015 |
| 分类号:R917 |
| 基金项目: |
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| Content Determination of Aristolochic Acid Analogs in Houttuynia Cordata and Compound Yuxincao Mixture by HPLC-MS/MS |
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MA Linke1, WANG Juanjuan1,2, ZHENG Cheng1,2
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1.Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China;2.NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine, Hangzhou 310052, China
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| Abstract: |
| OBJECTIVE To establish an HPLC-MS/MS method for simultaneous determination of aristolochic acid I, aristolochic acid II and aristolactam I in Houttuynia cordata and Compound Yuxincao mixture.METHODS Phenomenex Kinetex C18(100 mm×2.1 mm, 2.6 μm) column was used for separation. The mobile phase consisted of acetonitrile and 0.2% formic acid solution with gradient elution. The flow rate was 0.3 mL·min-1and the column temperature was 30℃. Electrospray positive ion source was used for mass spectrometry detection by multiple reaction monitoring mode. RESULTS The liner range of calibration curve was 11.91-1 985 ng·mL-1(r=0.995 3), 16.87-2 812 ng·mL-1(r=0.995 7) and 3.404-567.4 ng·mL-1(r=0.996 6) for aristolochic acid I, aristolochic acid II and aristolactam I. The average recoveries of each component was in the range of 85%-111%, RSD was 0.2%-6.7%. The limit of detection and quantitation for aristolochic acid I were 2.395 ng·mL-1 and 7.984 ng·mL-1, for aristolochic acid II were 3.389 ng·mL-1 and 10.50 ng·mL-1, and for aristolactam I were 0.334 2 ng·mL-1 and 1.113 ng·mL-1. CONCLUSION The method has good sprcificity, sensitivity and accuracy, and it is suitable for the content determination of aristolochic acid I, aristolochic acicl II and aristolactam I in Compound Yuxincao mixture. |
| Key words: Houttuynia cordata Compound Yuxincao mixture aristolochic acid analogs HPLC-MS/MS |
