液质联用法测定鹭鸶咯丸中马兜铃酸类成分  

Determination of Aristolochic Acids in Lusika Pills by Liquid Chromatography-mass Spectrometry

作　　者：谭乐俊 于新兰 林林 于凤蕊 牛艳 林永强 戴忠[3] TAN Le-jun;YU Xin-lan;LIN Lin;YU Feng-rui;NIU Yan;LIN Yong-qiang;DAI Zhong(Shandong Provincial Institute for Food and Drug Control,NMPA Key Laboratory for Quality Evaluation of Gelatin Products,Shandong Engineering Laboratory for Standard Innovation and Quality Evaluation of TCM,Shandong Engineering Research Center of Generic Technologies for Traditional Chinese Medicine Formula Granules,Jinan 250101,China;Xinjiang Uygur Autonomous Region Institute of Drug Control,Urumqi 830002,China;National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]山东省食品药品检验研究院国家药品监督管理局胶类产品质量评价重点实验室/山东省中药标准创新与质量评价工程实验室/中药配方颗粒共性技术山东省工程研究中心,山东济南250101 [2]新疆维吾尔自治区药品检验研究院,新疆乌鲁木齐830002 [3]中国食品药品检定研究院,北京100050

出　　处：《中国现代中药》2023年第9期1985-1991,共7页Modern Chinese Medicine

基　　金：山东省重点研发计划重大科技创新工程项目(2021CXGC010511);山东省重点研发计划项目(2020RKB24001);山东省人文社会科学课题(2021-YYGL-44)。

摘　　要：目的:为明确鹭鸶咯丸是否含有马兜铃酸Ⅰ等马兜铃酸类成分,建立其马兜铃酸类成分的液质联用检测分析方法。方法:采用岛津Shim-pack Velox C_(18)色谱柱(100 mm×2.1 mm,2.7μm),以甲醇-0.1%甲酸溶液(含5 mmol·L^(-1)甲酸铵)为流动相梯度洗脱;电喷雾正离子模式(ESI^(+)),多反应监测(MRM)模式,对鹭鸶咯丸中7个马兜铃酸类成分进行初步筛查,并建立3个马兜铃酸成分的液质联用检测方法。结果:15批鹭鸶咯丸样品中检出马兜铃酸Ⅰ(0.003~0.011μg·g^(-1))、马兜铃酸Ⅳa(0.169~0.260μg·g^(-1))和马兜铃内酰胺Ⅰ(0.036~0.169μg·g^(-1)),进样量在相应范围内线性关系良好(r≥0.999 9),平均加样回收率分别为96.1%(RSD为1.63%)、99.4%(RSD为1.27%)、96.4%(RSD为2.98%),精密度及方法重复性均良好。结论:所建立的方法准确、灵敏、可靠,可用于鹭鸶咯丸中7个马兜铃酸类成分的筛查,且可用于上述3个马兜铃酸成分的分析,可为鹭鸶咯丸的质量控制及其安全使用提供参考。Objective:To establish a method for the determination of aristolochic acids including aristolochic acidⅠin Lusika Pills with liquid chromatography-mass spectrometry(LC-MS).Methods:Shimadzu Shim-pack Velox C_(18) column(100 mm×2.1 mm,2.7μm)was used for the gradient elution with methanol-0.1%formic acid solution(containing 5 mmol·L^(-1) ammonium formate)as the mobile phase.The electrospray ionization in positive ion mode(ESI^(+))and multiple-reaction monitoring(MRM)mode were used for initially screening of 7 aristolochic acids.Furthremore,the LC-MS method was established to detect 3 aristolochic acids.Results:Aristolochic acidⅠ(0.003-0.011μg·g^(-1)),aristolochic acidⅣa(0.169-0.260μg·g^(-1)),and aristololactamⅠ(0.036-0.169μg·g^(-1))were detected in all the 15 batches of samples.The established method showed good linearity within the corresponding range(r≥0.9999).The average recovery of the three components was 96.1%(RSD of 1.63%),99.4%(RSD of 1.27%),and 96.4%(RSD of 2.98%),respectively.The established method showed good precision and repeatability. Conclusion: The established method is accurate, sensitive, and reliable and can be applied to the screening of aristolochic acids and determination of the above three components in Lusika Pills. The findings can provide a scientific basis for the quality control and safe application of Lusika Pills.

关 键 词：鹭鸶咯丸 液质联用 马兜铃酸Ⅰ 马兜铃酸Ⅳa 马兜铃内酰胺Ⅰ 安全性 

分 类 号：R286[医药卫生—中药学]