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

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，2.5 μm），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>0.998 5），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、0.03~41.47 μg·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,2.5 μm),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 0.03-41.47 μg 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.

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