基于RRLC-QQQ-MS/MS法的清火栀麦片中4个有效成分同时测定及湖北麦冬的检查

Simultaneous determination of four active components and detection of Liriope spicata in Qinhuo Zhimai tablets by RRLC-QQQ-MS/MS

目的:建立同时测定清火栀麦片中4个指标成分(脱水穿心莲内酯、穿心莲内酯、栀子苷、麦冬皂苷D)并检查湖北麦冬的方法。方法:应用超高效液相色谱-三重四极杆串联质谱(RRLC-QQQ MS/MS)技术,采用岛津XBridge BEH C18色谱柱(2.1 mm×100 mm,2.5μm),以0.1%乙酸水溶液(含10 mmol·L^-1乙酸铵)-乙腈为流动相,梯度洗脱,流速0.3 mL·min^-1,柱温35℃,采用电喷雾离子源(ESI),以多反应监测(MRM)模式进行正、负离子同时扫描。结果:5个成分在相应线性范围内线性关系良好(r>0.9985),平均加样回收率为92.9%~99.3%,RSD均小于4.6%。10批样品中脱水穿心莲内酯、穿心莲内酯、栀子苷、麦冬皂苷D的含量范围分别为526.93~1206.23、135.05~812.00、349.66~958.64、0.03~41.47μg·片^-1;有3批检出湖北麦冬,均来自不同厂家。结论:建立的方法能快速测定清火栀麦片中的4个成分的含量,并筛查制剂中是否掺加湖北麦冬。

Objective:To establish a method for the simultaneous determination of four active components(dehydroandrographolide,andrographolide,geniposide and ophiopogonin D)in Qinhuo Zhimai tablets and detection of Liriope spicata.Methods:The rapid resolution liquid chromatography coupled with triple quadruple mass spectrometry(RRLC-QQQ-MS/MS)was performed.The chromatographic separation was achieved on Shimadzu XBridge BEH C18(2.1 mm×100 mm,2.5μm),with the mobile phase comprising of 0.1%acetic acid(containing 10 mmol·L^-1 ammonium acetate)solution-acetonitrile flowing at 0.3 mL·min^-1 in a gradient elution manner.The column temperature was 35℃.The analytes were detected by tandem mass spectrometry with electrospray ionization(ESI)source,and scanned by ESI±multiple reaction monitoring(MRM)mode.Results:Five components showed good linear relationships within their own ranges(r>0.9985),whose average recoveries were ranged from 92.9%to 99.3%(RSD<4.6%).The contents of dehydroandrographolide,andrographolide,geniposide and ophiopogonin D in 10 batches of samples were 526.93-1206.23,135.05-812.00,349.66-958.64 and 0.03-41.47μg per tablet,respectively.Liriope spicata was detected in 3 out of 10 samples from different manufacturers.Conclusion:The method can simultaneously determine four active components in Qinhuo Zhimai tablets,and screening whether Liriope spicata is blended.