高效液相色谱-串联质谱法测定天王补心丸中山麦冬
李丽莉，吕轶峰，宁崇良，覃丽郦，白桂昌，何颂华
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
Determination of Liriopes Radix in Tianwang Buxin pills by high performance liquid chromatography-tandem mass spectrometry
LI Lili, LYU Yifeng, NING Chongliang, QIN Lili, BAI Guichang, He Songhua
Guangxi Institute for Food and Drug Control, Nanning 530021, China
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、5.2～2 080 ng/mL 范围内与色谱峰面积线性关系良好，相关系数均为 0.999 3，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。
Abstract：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% 18 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 5.2-2 080 ng/mL, respectively, the correlation coefficients were all 0.999 3, 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
Keywords：ultra high performance liquid chromatography tandem mass spectrometry; Tianwang Buxin pills;Ophiopogonis Radix; Liriopes Radix; Liriopesides B; liriope muscari baily saponins C
本文引用格式：
李丽莉，吕轶峰，宁崇良，等.高效液相色谱-串联质谱法测定天王补心丸中山麦冬[J].化学分析计量，2023，32(10)：72.
LI Lili，LYU Yifeng，NING Chongliang，et al. Determination of Liriopes Radix in Tianwang Buxin pills by high performance liquidchromatography-tandem mass spectrometry[J]. Chemical Analysis and Meterage，2023，32(10)：72.
相似文章：
