超高效液相-质谱法测定滴通鼻炎水中马兜铃酸Ⅰ、Ⅱ的含量  

Content determination of aristolochic acidⅠand aristolochic acidⅡin Ditong Biyan Shui by UPLC-MS/MS

作　　者：郭日新 肖萌 刘静[1] 戴忠[1] 马双成[1] GUO Rixin;XIAO Meng;LIU Jing;DAI Zhong;MA Shuangcheng(Institute for Control of Chinese Traditional Medicine and Ethnic Medicine,National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院中药民族药检定所,北京100050

出　　处：《中国药物警戒》2024年第4期386-390,396,共6页Chinese Journal of Pharmacovigilance

基　　金：国家科技重大专项重大新药创制(2018ZX09735-006);2022年度国家药品标准制修订研究课题(2022Z16);国家药品监督管理局药品监管科学体系建设重点项目(RS2024Z006)。

摘　　要：目的测定滴通鼻炎水中马兜铃酸Ⅰ、马兜铃酸Ⅱ的含量,为其质量控制提供借鉴。方法采用超高效液相-质谱法(UPLC-MS/MS)同时测定滴通鼻炎水中马兜铃酸Ⅰ、马兜铃酸Ⅱ的含量。色谱柱采用Waters-ACQUI UPLC HSS T3 C_(18)(2.1 mm×100 mm,1.8μm),采用乙腈为流动相A,0.1%甲酸含1 mmol·L^(-1)乙酸铵溶液为流动相B,梯度洗脱,电喷雾离子源(ESI),正离子多反应监测模式,以标准曲线法计算含量。结果17批滴通鼻炎水中有9批样品未检出马兜铃酸Ⅰ(检出限0.13 pg),8批样品中检出马兜铃酸Ⅰ,含量在0.41~3.60 ng·mL^(-1)。所有样品中均未检出马兜铃酸Ⅱ(检出限0.41 pg)。结论建立了UPLC-MS/MS同时测定滴通鼻炎水中马兜铃酸Ⅰ、马兜铃酸Ⅱ含量的方法,该方法专属性强、灵敏度高、重复性好,可为滴通鼻炎水中马兜铃酸Ⅰ、马兜铃酸Ⅱ的质量控制提供参考。Objective To determine the contents of aristolochic acid I and aristolochic acidⅡin Ditong Biyan Shui,and to provide reference for quality control.Methods A UPLC-MS/MS method was established to determine the contents of aristolochic acid I and aristolochic acidⅡ.An Waters-ACQUI UPLC HSS T3 C_(18)(2.1 mm×100 mm,1.8μm)was used as the chromatographic column.The mobile phase was eluted with acetonitrile(A),0.1%formic acid solution(B)using a gradient elution method.The electrospray spray ion source(ESI)and positive ion multi-reaction monitoring mode were adopted.The contents were calculated using the standard curve method.Results Aristolochic acid I was not detected in 9 samples of 17 batches of Ditong Biyan Shui(detection limit 0.13 pg),but was detected in 8 batches of samples,with the contents ranging from 0.41 to 3.60 ng·mL^(-1).Aristolochic acidⅡwas not detected in any of the samples(detection limit 0.41 pg).Conclusion A UPLC-MS/MS method has been established to determine the contents of aristolochic acid I and aristolochic acidⅡin Ditong Biyan Shui,with high specificity,high sensitivity,good repeatability,which can provide reference for quality control of aristolochic acid I and aristolochic acidⅡin Ditong Biyan Shui.

关 键 词：滴通鼻炎水 马兜铃酸Ⅰ 马兜铃酸Ⅱ 超高效液相-质谱法 含量测定 

分 类 号：R927.1[医药卫生—药学]