UPLC-QQQ MS法评价川贝雪梨膏中麦冬投料掺伪情况

Assessment of Adulteration of Ophiopogon Radix Feeding in Chuanbei Xueli Ointments by UPLC-QQQ MS

目的分析川贝雪梨膏中麦冬的投料情况,建立川贝雪梨膏中掺杂山麦冬的专属性检测方法。方法采用甲醇-氨水对川贝雪梨膏进行提取,利用超高效液相色谱-三重四极杆质谱对麦冬成分进行检测。采用Agilent Zorbax Eclipse-C_(18)色谱柱(2.1 mm×100 mm,1.5μm),以乙腈(A)-15 mmol·L^(-1)乙酸铵溶液(B)为流动相,梯度洗脱;流速:0.35 ml·min^(-1);柱温:35℃;进样量:2μl;选择山麦冬皂苷B离子峰m/z 723.4(双电荷)→251.2、269.2及短葶山麦冬皂苷C离子峰m/z 893.5(双电荷)→463.1、481.2作为检测离子对,离子化模式为ESI+,进行多反应监测。结果9批市售川贝雪梨膏样品中均未检出掺杂山麦冬成分。结论本研究建立的方法专属性强、准确可靠,可以用于判断市售川贝雪梨膏中麦冬的投料掺伪情况。

Objective To establish a method for identification of Ophiopogonis Radix in Chuanbei Xueli ointments by studying the quality of the feeding.Methods Chuanbei Xueli ointments were extracted with methanol-ammonia while the content of Ophiopogonis Radix was detected with rapid resolution liquid chromatography(UPLC)coupled to triple quadruple mass spectrometry(QQQ MS).Determination was carried out on an Agilent Zorbax Eclipse-C_(18)(2.1 mm×100 mm,1.5μm)column with a column temperature of 35℃.The mobile phase was composed of acetonitrile(A)-15 mmol·L^(-1) ammonium acetate(B)under gradient elution at a flow rate of 0.35 ml·min^(-1),and the injection volume was 2μl.The characteristic ion pairs of liriopeside B m/z 723.4(double charge)→251.2,269.2 and those of Liriope muscari baily saponin C m/z 893.5(double charge)→463.1,481.2 were selected as detection ion pairs.Positive electrospray ionization and multiple reaction monitoring were adopted.Results No adulteration of Ophiopogonis Radix was detected in 9 batches of commercial Chuanbei Xueli ointments.Conclusion The established method is specific,accurate and reliable,which can be used to assess adulteration of Ophiopogonis Radix in Chuanbei Xueli ointments.