基于HPLC-Q-TOF-MS技术检测川贝清肺糖浆中掺伪山麦冬的研究

Detection of Liriopes Radix Adulterated in ChuanBei QingFei Syrup by HPLC-Q-TOF-MS

目的采用高效液相色谱-四级杆串联飞行时间质谱(HPLC-Q-TOF-MS)技术建立川贝清肺糖浆中掺伪山麦冬的检测方法。方法采用色谱柱Agilent Po roshell 120 EC-C_(18)(50 mm×4.6 mm,2.7μm),流动相为乙腈-0.1%冰醋酸(50∶50),流速为0.3 mL·min^(-1),柱温为35℃;电喷雾电离(ESI-),以麦冬皂苷D、山麦冬皂苷B和短葶山麦冬皂苷C为指标性成分进行分析。结果50批样品中有6批检出山麦冬皂苷B和麦冬皂苷D,应为掺山麦冬(湖北麦冬)投料;有4批均未检出3种指标性成分,疑似未使用麦冬投料。结论该方法专属性强,灵敏度高,可用于对川贝清肺糖浆中掺伪山麦冬的检查。

OBJECTIVE To establish method for the determination of Liriopes Radix Adulterated in ChuanBeiQingFei Syrup by HPLC-Q-TOF-MS.METHODS Agilent Poroshell 120 EC-C_(18) chromatographic column(50 mm×4.6 mm,2.7μm)was employed and the separation was performed with the mobile phase consisting of acetonitrile-0.1% glacial acetic acid aqueous solution(50∶50)at a flow rate of 0.3 mL·min^(-1).The column temperature was 35℃ and the mass spectrometry was conducted in negative ion mode with electrospray ionization(ESI).And Ophiopogonin D,Liriopesides B and Liriope muscari baily saponins C were used as the index components for analysis.RESULTS In 50 batches of samples,6 batches which were detected Ophiopogonin D and Liriopesides B,mixed with Liriopes Radix(Liriope spicata(Thunb.)Lour.var.prolifera Y.T.Ma),and 4 batches that were not detected the three index components were suspected of delivering without Ophiopogonis Radix.CONCLUSION The method which has significant advantages such as high specificity and sensitivity,can be applied to detection of Liriopes Radix adulterated in ChuanBei QingFei Syrup.