天王补心丸中炒酸枣仁掺伪情况的研究  

Adulteration situation of fried Ziziphi Spinosae Semen in Tianwang Buxin pills

作　　者：李丽莉 吕轶峰 张慧 叶倩 宁崇良 何颂华 罗轶 LI Li-li;LU Yi-feng;ZHANG Hui;YE Qian;NING Cong-ling;HE Song-hua;LUO Yi(Guangxi Institute for Food and Drug Control,NMPA Key Laboratory for Quality Monitor and Evaluation of Traditional Chinese Medicine,Chinese Material Medica,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：《药物分析杂志》2023年第4期693-700,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立天王补心丸中炒酸枣仁的混淆品炒理枣仁的检查方法,测定127批天王补心丸(水蜜丸、大蜜丸)样品,以考察样品中炒酸枣仁的投料状况,予相关生产企业及监管部门警示。方法:应用高分离度快速液相色谱-三重串联四极杆质谱(UPLC-QQQ/MS)技术,采用Agilent Eclipse C18(100 mm×2.1 mm,1.8μm)色谱柱,以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,流速0.2 mL·min^(-1),柱温30℃,进样量1μL;采用电喷雾离子源(ESI),以多反应监测(MRM)模式进行正离子扫描。结果:在所设立的色谱条件下,欧鼠李叶碱在相应线性范围内线性关系良好(r>0.999),水蜜丸与大蜜丸中欧鼠李叶碱的加样回收率(n=9)分别为99.13%、97.16%,RSD均<3.3%。用所建立的方法测定127批天王补心丸样品,检出炒理枣仁15批。结论:天王补心丸中存在以炒理枣仁代替炒酸枣仁投料的情况。Objective:To establish the detection method of fried Ziziphi Mauritianae Semen in Tianwang Buxin pills to uncover the adulteration situation of fried Ziziphi Spinosae Semen in Tianwang Buxin pills.Methods:The rapid resolution liquid chromatography coupled with triple quadruple mass spectrometry(RRLC-QQQ/MS)was used.The chromatographic separation was achieved on an Agilent Eclipse C_(18)Column(100 mm×2.1 mm,1.8μm),with the mobile phase comprising of 0.1%formic acid solution and acetonitrile at a flow rate of 0.2 mL·min^(-1)in a gradient elution manner.The column temperature was 30℃.The analytes were detected by tandem mass spectrometry with electrospray ionization(ESI)source,and scanned by ESI^(+)multi-reaction monitoring(MRM)mode.Results:Frangufoline showed good linear relationships within their own ranges(r>0.999).The recoveries of water honey pills and big honey pills were 99.13%and 97.16%(RSD<3.3%,n=9).The method was used to determine 127 batches of Tian Wang Bu Xin Dan samples and fried semen ziziphi spinosae were detected in 15 batches of samples.Conclusion:The mixture of fried Ziziphi Spinosae Semen with Fried Ziziphi Mauritianae Semen exists in Tianwang Buxin pills.

关 键 词：天王补心丸 炒酸枣仁 掺伪 炒理枣仁 欧鼠李叶碱 高分离度快速液相色谱-三重串联四极杆质谱 

分 类 号：R917[医药卫生—药物分析学]