{"title":"超高效液相色谱-三重四极杆串联质谱法快速同时测定细辛中6种马兜铃酸和2种木脂素","authors":"Hanze Liu, Huida Guan, Xue Cheng, Changhong Wang","doi":"10.2139/ssrn.3874499","DOIUrl":null,"url":null,"abstract":"Asari Radix et Rhizoma (AR) is a well-known Chinese herbal medicine which has been used to treat cold headache, toothache, runny nose, rhinorrhea, rheumatism and cough in China. However, the existing Pharmacopoeia standard of AR is still unable to comprehensively evaluating the overall efficacy and safety of AR, whose traditional HPLC detection method has great limitations for the detection of trace aristolochic acids. In order to improving the quality control method of AR, a rapid, simple, and reliable chromatographic analytic method based on ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-QQQ-MS) was established for the analysis of 8 target compounds, including 6 aristolochic acids derivates aristolochic acid (AA)-I, AA-II, AA-III, AA-IVa, AA-VIIa, aristololactam I (AL-I), and 2 lignans asarinin and sesamin. Chromatographic separation has been achieved on an ACQUITY UPLC BEH C18 column (50 mm × 2.1 mm, id 1.8 μm) with a mobile phase consisted of water containing 0.1% formic acid (A) and acetonitrile (B) with gradient elution manner. Positive electrospray ionization mode with multiple reaction monitoring (MRM) was applied for the detection of the eight analytes. Method validation results indicated that UPLC-QQQ-MS was precise, accurate and sensitive for quantitative determination of the eight analytes. Finally, the method was successfully used to the analysis of each component in 15 batches of AR herb samples. In addition to existing marker ingredients AA-I and asarinin, considerable amounts of AA-IVa, AA-VIIa, AL-I and sesamin were also found in each AR sample. The result suggesting that AA-IVa, AA-VIIa, AL-I should be limited and sesamin should be added as a quality marker for the quality control of AR.","PeriodicalId":19880,"journal":{"name":"PharmSciRN EM Feeds","volume":"11 1","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Rapid and Simultaneously Determination of Six Aristolochic Acids and Two Lignans in Asari Radix Et Rhizoma by Ultra Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry\",\"authors\":\"Hanze Liu, Huida Guan, Xue Cheng, Changhong Wang\",\"doi\":\"10.2139/ssrn.3874499\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"Asari Radix et Rhizoma (AR) is a well-known Chinese herbal medicine which has been used to treat cold headache, toothache, runny nose, rhinorrhea, rheumatism and cough in China. However, the existing Pharmacopoeia standard of AR is still unable to comprehensively evaluating the overall efficacy and safety of AR, whose traditional HPLC detection method has great limitations for the detection of trace aristolochic acids. In order to improving the quality control method of AR, a rapid, simple, and reliable chromatographic analytic method based on ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-QQQ-MS) was established for the analysis of 8 target compounds, including 6 aristolochic acids derivates aristolochic acid (AA)-I, AA-II, AA-III, AA-IVa, AA-VIIa, aristololactam I (AL-I), and 2 lignans asarinin and sesamin. Chromatographic separation has been achieved on an ACQUITY UPLC BEH C18 column (50 mm × 2.1 mm, id 1.8 μm) with a mobile phase consisted of water containing 0.1% formic acid (A) and acetonitrile (B) with gradient elution manner. Positive electrospray ionization mode with multiple reaction monitoring (MRM) was applied for the detection of the eight analytes. Method validation results indicated that UPLC-QQQ-MS was precise, accurate and sensitive for quantitative determination of the eight analytes. Finally, the method was successfully used to the analysis of each component in 15 batches of AR herb samples. In addition to existing marker ingredients AA-I and asarinin, considerable amounts of AA-IVa, AA-VIIa, AL-I and sesamin were also found in each AR sample. The result suggesting that AA-IVa, AA-VIIa, AL-I should be limited and sesamin should be added as a quality marker for the quality control of AR.\",\"PeriodicalId\":19880,\"journal\":{\"name\":\"PharmSciRN EM Feeds\",\"volume\":\"11 1\",\"pages\":\"\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2021-01-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"PharmSciRN EM Feeds\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.2139/ssrn.3874499\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"PharmSciRN EM Feeds","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.2139/ssrn.3874499","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 0
摘要
细辛是一种著名的中草药,在中国被用来治疗感冒、头痛、牙痛、流鼻涕、鼻漏、风湿病和咳嗽。然而,现有的AR药典标准仍无法全面评价AR的整体功效和安全性,其传统的HPLC检测方法对痕量马兜铃酸的检测存在很大的局限性。为了改进AR的质量控制方法,建立了一种基于超高效液相色谱-三重四极杆串联质谱(UPLC-QQQ-MS)的快速、简便、可靠的色谱分析方法,对马兜铃酸衍生物马兜铃酸(AA)-I、AA- ii、AA- iii、AA- iva、AA- viia、马兜铃内酯I (AL-I)、木脂素asarinin和sesamin等8个目标化合物进行分析。采用ACQUITY UPLC BEH C18色谱柱(50 mm × 2.1 mm, id 1.8 μm),流动相为含有0.1%甲酸(a)和乙腈(B)的水,梯度洗脱。采用多反应监测的正电喷雾电离模式(MRM)对8种分析物进行检测。方法验证结果表明,UPLC-QQQ-MS方法精密度高、准确度高、灵敏度高。最后,该方法成功应用于15批AR药材样品中各成分的分析。在每个AR样品中,除了现有的标记成分AA-I和细辛素外,还发现了相当数量的AA-IVa、AA-VIIa、AL-I和芝麻素。结果提示,应限制AA-IVa、AA-VIIa、AL-I的含量,并添加芝麻素作为质量标记物对AR进行质量控制。
Rapid and Simultaneously Determination of Six Aristolochic Acids and Two Lignans in Asari Radix Et Rhizoma by Ultra Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry
Asari Radix et Rhizoma (AR) is a well-known Chinese herbal medicine which has been used to treat cold headache, toothache, runny nose, rhinorrhea, rheumatism and cough in China. However, the existing Pharmacopoeia standard of AR is still unable to comprehensively evaluating the overall efficacy and safety of AR, whose traditional HPLC detection method has great limitations for the detection of trace aristolochic acids. In order to improving the quality control method of AR, a rapid, simple, and reliable chromatographic analytic method based on ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-QQQ-MS) was established for the analysis of 8 target compounds, including 6 aristolochic acids derivates aristolochic acid (AA)-I, AA-II, AA-III, AA-IVa, AA-VIIa, aristololactam I (AL-I), and 2 lignans asarinin and sesamin. Chromatographic separation has been achieved on an ACQUITY UPLC BEH C18 column (50 mm × 2.1 mm, id 1.8 μm) with a mobile phase consisted of water containing 0.1% formic acid (A) and acetonitrile (B) with gradient elution manner. Positive electrospray ionization mode with multiple reaction monitoring (MRM) was applied for the detection of the eight analytes. Method validation results indicated that UPLC-QQQ-MS was precise, accurate and sensitive for quantitative determination of the eight analytes. Finally, the method was successfully used to the analysis of each component in 15 batches of AR herb samples. In addition to existing marker ingredients AA-I and asarinin, considerable amounts of AA-IVa, AA-VIIa, AL-I and sesamin were also found in each AR sample. The result suggesting that AA-IVa, AA-VIIa, AL-I should be limited and sesamin should be added as a quality marker for the quality control of AR.