摘要
目的:建立高效液相色谱-二极管阵列检测器-蒸发光检测器法(HPLC-PDAELSD)和超高效液相色谱-质谱法(UPLC-MS/MS)考察抗菌消炎胶囊(片)中大黄和金银花投料的有效性。方法:以华北大黄的特征成分土大黄苷和山银花的特征成分灰毡毛忍冬皂苷乙为检测指标,采用HPLC-PDA-ELSD法检查,色谱柱为CAPCELLPAKC18(4.6 mm×250 mm,5μm);流动相为乙腈-水,梯度洗脱;流速为1.0 mL·min^(-1);PDA检测波长为324 nm;蒸发光散射检测器条件:漂移管温度为75℃,气体压力为172 kPa。采用UPLC-MS/MS法对结果进行定性验证,以m/z419.0→257.1和m/z419.0→241.0作为土大黄苷检测离子对,以m/z1 397.3→1 073.3和m/z1 397.3→471.4作为灰毡毛忍冬皂苷乙检测离子对,电喷雾负离子模式(ESI-),多反应监测(MRM)。结果:11批次样品中,有1批次检出有土大黄苷,2批次检出灰毡毛忍冬皂苷乙,说明该品种大黄和金银花的投料存在不规范的情况。结论:建立的方法专属性强,结果准确可靠,重现性好,可有效监测抗菌消炎胶囊(片)中大黄和金银花的投料情况。
Objective:To establish HPLC-PDA-ELSD and UPLC-MS/MS methods for simultaneous determination of rhaponticin(a characteristic component of Rheum franzenbachii Munt.)and macranthoidin B(a characteristic component of Lonicera confusa DC.),to investigate the phenomenon of illegal feeding in Kangjunxiaoyan Capsules(Tablets).Methods:HPLC-PDA-ELSD was used to determine rhaponticin and macranthoidin B as the indexes of illegal feeding.The positive samples were verified by UPLC-MS/MS.The chromatographic column was CAPCELL PAK C18(4.6 mm×250 mm,5μm).The mobile phase was acetonitrile and water for gradient elution.The flow rate was 1.0 mL·min^(-1).The PDA detection wave-length was 324 nm.For evaporative light scattering detection,the drift tube temperature was 75℃ and the gas pressure was 172 kPa.An UPLC-MS/MS method was used to qualitatively verify the results.The elec-trospray negative ion mode(ESI-)and multi reaction monitoring(MRM)were used with m/z 419.0→257.1 and m/z 419.0→241.0 as the detection ion pairs of rhaponticin and m/z 1397.3→1073.3 and m/z 1397.3→471.4 as the detection ion pairs of macranthoidin B.Results:Among the 11 batches of samples,rhaponti-cin was detected in 1 batch and macranthoidin B was detected in 2 batches,indicating that the feeding of these Kangjunxiaoyan Capsules(Tablets)were not standardized.Conclusion:The established method is specific,accurate reliable and reproducible,and can effectively monitor the feeding of Rhei Radix et Rhi-zoma and Lonicerae Japonicae Flos in Kangjunxiaoyan Capsules(Tablets).
作者
吴琦
贾银芝
张水红
刘益庆
赵猛
佟悦
WU Qi;JIA Yinzhi;ZHANG Shuihong;LIU Yiqing;ZHAO Meng;TONG Yue(Lianyungang Food and Drug Inspection Center,Lianyungang 222006,China;Lianyungang Laboratory of Jiangsu Institute for Food and Drug Control,Lianyungang 222006,China)
出处
《药学与临床研究》
2025年第1期49-53,共5页
Pharmaceutical and Clinical Research
基金
江苏省市场监督管理局科技计划项目(KJ2025078)。
