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作 者:刘益庆 吴琦 赵猛 陈洪岩 钱明明 李玲 LIU Yiqing;WU Qi;ZHAO Meng;CHEN Hongyan;QIAN Mingming;LI Ling(Lianyungang Inspection Testing Center of Food and Drug,Lianyungang 222006,China)
机构地区:[1]连云港市食品药品检验检测中心,连云港222006
出 处:《药学与临床研究》2023年第3期234-237,共4页Pharmaceutical and Clinical Research
基 金:2021年江苏省市场监督管理局科技计划项目(KJ21125046)。
摘 要:目的:建立银翘解毒片中掺伪山银花成分灰毡毛忍冬皂苷乙和川续断皂苷乙的检测方法。方法:采用高效液相色谱-电喷雾检测器法(HPLC-CAD),色谱柱为Superiorex ODS C18(250 mm×4.6 mm,5μm),乙腈-水为流动相梯度洗脱,流速为1.0 mL·min^(-1),雾化器温度45℃,采集频率10 Hz,滤光片10.0 s,并对检出的掺伪山银花采用高效液相色谱-质谱联用方法确认。结果:灰毡毛忍冬皂苷乙在0.239~7.158μg内呈良好线性关系,r=0.9992(n=7),平均回收率为99.43%,RSD=0.94%(n=9);川续断皂苷乙在0.202~6.066μg内呈良好线性关系,r=0.9993(n=7),平均回收率为98.86%,RSD=0.76%(n=9)。结论:该方法科学、准确,适用于银翘解毒片中掺伪山银花,以检查保证用药安全。Objective:To establish a method for the detection of adulterated lonicera hypoglauca and dipsacoside B in Yinqiaojiedu tablets.Methods:An HPLC-CAD method was used with Superiorex ODS C18(250 mm×4.6 mm,5μm)as the analytical column,acetonitrile was used as mobile phase A and water as mobile phase B for gradient elution,the flow rate was 1.0 mL·min^(-1),the atomizer temperature was 45°C,the collection frequency was 10 Hz,the filter was 10.0 s,and the adulterated Lonicera hypoglauca detected was confirmed by HPLC-MS/MS.Results:The linear range of macranthoidin B was 0.239-7.158μg,r=0.9992(n=7),the average recovery of macranthoidin B was 99.43%,with RSD 0.94%(n=9),the linear range of dipsacoside B was 0.202-6.066μg,r=0.9993(n=7),the average recovery of dipsacoside B was 98.86%,with RSD 0.76%(n=9).Conclusion:The method is scientific and accurate,and is applicable to the inspection of lonicerae hypoglaucae flos in Yinqiaojiedu tablets,so as to tnsure sofety drug.
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