超高效液相色谱–串联质谱法检测玄麦甘桔颗粒中山麦冬的含量  

Determination of Liriope spicata(Thunb.)Lour.content in Xuanmai Ganju Granules by ultra-high performance liquid chromatography tandem mass spectrometry

作　　者：袁林 万莉 张德伟 陈爽 YUAN Lin;WAN Li;ZHANG De-Wei;CHEN Shuang(Chongqing Wanzhou Food and Drug Inspection Institute,Chongqing 404100,China;Chongqing Key Laboratory of Development and Utilization of Genuine Medicinal Materials in the Three Gorges Reservoir Area,Chongqing 404100,China;Chongqing Engineering Laboratory of Green Planting and Deep Pocessing of Genuine Medicinal Materials in the Three Gorges Reservoir Area,College of Biological and Food Engineering,Chongqing Three Gorges University,Chongqing 404120,China)

机构地区：[1]重庆市万州食品药品检验所,重庆404100 [2]三峡库区道地药材开发利用重庆市重点实验室,重庆404100 [3]重庆三峡学院生物与食品工程学院,三峡库区道地药材绿色种植与深加工重庆市工程实验室,重庆404120

出　　处：《实验室检测》2024年第11期1-6,共6页Laboratory Testing

基　　金：重庆市药品监督管理局、重庆市科学技术局项目——玄麦甘桔类制剂中山麦冬检查项补充检验方法(渝药监[2022]27号)

摘　　要：目的建立超高效液相色谱–三重四级杆串联质谱(UPLC-MS/MS)法同时测定玄麦甘桔颗粒中麦冬特征成分和湖北麦冬特征成分山麦冬皂苷B与短葶山麦冬特征成分短葶山麦冬皂苷C的含量。方法玄麦甘桔颗粒采用甲醇超声提取后,分析采用OMNI Orca C_(18)色谱柱(2.1 mm×100 mm,2.6μm),流动相采用10 mmol/L乙酸铵溶液和甲醇进行梯度洗脱,色谱柱温度设置为40℃,进样量为1μL,使用电喷雾离子源(ESI),正负离子同时扫描模式,多反应监测模式,测定麦冬中成分甲基麦冬黄烷酮A、甲基麦冬黄烷酮B,以及掺伪品湖北麦冬中的山麦冬皂苷B、短葶山麦冬中的短葶山麦冬皂苷C的含量。结果甲基麦冬黄烷酮A、甲基麦冬黄烷酮B、山麦冬皂苷B和短葶山麦冬皂苷C在各自的范围内线性关系良好,r均大于0.996,回收率范围为90.6%~99.8%。结论该方法前处理简便快捷、灵敏度高、结果准确可靠,可以用于判断市售玄麦甘桔颗粒中麦冬掺伪山麦冬的投料情况及为监管部分提供执法依据。Objective To establish an ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)method for simultaneous determination of the characteristic components of Ophiopogon japonicus and Liriope spicata(Thunb.)Lour.var.prolifera Y.T.Ma saponins B and Liriope muscari(Decne.)Baily saponins C in Xuanmai Ganju granules.Methods Xuanmai Ganju Granules were extracted by methanol ultrasound and analyzed using OMNI Orca C_(18) chromatography column(2.1 mm×100 mm,2.6μm).The mobile phase was eluted using a gradient elution of 10 mmol/L ammonium acetate solution and methanol.The column temperature was set to 40℃,and the injection amount was 1μL.The contents of methyl ophiopogon flavanone A and methyl ophiopogon flavanone B in Ophiopogon japonicus,as well as saponin B in Liriope spicata(Thunb.)Lour.var.prolifera Y.T.Ma and saponin C in Liriope muscari(Decne.)Baily,using an electrospray ion source(ESI),a simultaneous scanning mode of positive and negative ions,and a multi reaction monitoring mode.Results Methyl ophiopogon flavanone A,methyl ophiopogon flavanone B,saponin B from Liriope spicata(Thunb.)Lour.var.prolifera Y.T.Ma,and saponin C from Liriope muscari(Decne.)Baily have good linear relationships within their respective ranges,with r values greater than 0.996 and recovery rates ranging from 90.6%to 99.8%.Conclusion This method has the advantages of simple and fast pre-treatment,high sensitivity,and accurate and reliable results.It can be used to determine the feeding situation of Ophiopogon japonicus mixed with Liriope spicata(Thunb.)Lour.in commercially available Xuanmai Ganju Granules and provide legal basis for regulatory authorities.

关 键 词：玄麦甘桔颗粒 超高效液相色谱–三重四级杆串联质谱 麦冬 山麦冬 

分 类 号：R286.0[医药卫生—中药学] O657.63[医药卫生—中医学]