高效液相色谱-串联质谱法测定天王补心丸中山麦冬  

Determination of Liriopes Radix in Tianwang Buxin pills by high performance liquid chromatography-tandem mass spectrometry

作　　者：李丽莉 吕轶峰 宁崇良 覃丽郦 白桂昌 何颂华 LI Lili;LYU Yifeng;NING Chongliang;QIN Lili;BAI Guichang;He Songhua(Guangxi Institute for Food and Drug Control,Nanning 530021,China)

机构地区：[1]广西壮族自治区食品药品检验所,国家药品监督管理局中药材质量监测与评价重点实验室,南宁530021

出　　处：《化学分析计量》2023年第10期72-76,共5页Chemical Analysis And Meterage

摘　　要：建立超高效液相色谱-串联质谱(HPLC-MS/MS)法测定天王补心丸中麦冬的混淆品山麦冬(湖北麦冬、短葶山麦冬)的方法。样品经甲醇提取,以0.1%(体积分数)甲酸-乙腈为流动相,用Waters CORTECS®C18色谱柱分离,采用电喷雾离子源(ESI),以多反应监测(MRM)模式进行正、负离子同时扫描,用HPLC-MS/MS法测定湖北麦冬、短葶山麦冬的代表性成分山麦冬皂苷B、短葶山麦冬皂苷C。山麦冬皂苷B、短葶山麦冬皂苷C的质量浓度分别在5.18~207.4、5.2~2080 ng/mL范围内与色谱峰面积线性关系良好,相关系数均为0.9993,方法检出限分别为56、134 ng/g。样品加标回收率分别为99.16%、101.54%,测定结果的相对标准偏差分别为2.57%、5.27%(n=9)。该方法简单、稳定、可靠,可用于分析天王补心丸中麦冬的掺假情况。A method for the determination of Liriopes(Liriope spicata and Radix Liriopes Muscari)in Tianwang Buxin pills by ultra high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was established.The samples were extracted with methanol and separated by Waters CORTECS®C18 chromatographic colunm with 0.1%formic acid solution-acetonitrile as the mobile phase.The electrospray ion source(ESI)was used to scan the positive and negative ions simultaneously in the multi reaction monitoring(MRM)mode,and Liriopesides B and liriope muscari baily saponins C which were the representative components of Liriopes were determined by HPLC-MS/MS.The mass concentrations of Liriopesides B and liriope muscari baily saponins C had a good linear relationship with the chromatographic peak area in the range of 5.18-207.4 and 5.2-2080 ng/mL,respectively,the correlation coefficients were all 0.9993,and the detection limits of the method were 56 and 134 ng/g,respectively.The recoveries of standard addition of the sample were 99.16%and 101.54%for Liriopesides B and liriope muscari baily saponins C,respectively,and the relative standard deviations of the determination results were 2.57%and 5.27%(n=9)for Liriopesides B and liriope muscari baily saponins C,respectively.The method is simple,stable and reliable,which is suitable for analysis the adulteration of Ophiopogonis Radix in Tianwang Buxin pills.

关 键 词：高效液相色谱-串联质谱法 天王补心丸 麦冬 山麦冬 山麦冬皂苷B 短葶山麦冬皂苷C 

分 类 号：O657.7[理学—分析化学]