LC-MS/MS法测定中成药制剂中23个非甾体抗炎药

目的: 建立了一种液相色谱串联四极杆质谱分析方法,对治疗风湿和类风湿的中成药制剂中的23个非甾体抗炎药进行快速筛查、定性识别和准确定量。 方法: 添加在中成药中的对乙酰氨基酚、乙酰水杨酸、安乃近、安替比林、洛索洛芬钠、氨基比林、吡罗昔康、萘普生、舒林酸、美洛昔康、氯唑沙宗、芬布芬、布洛芬、双氯芬酸、吲哚美辛、贝诺脂、尼美舒利、塞来昔布、醋氯芬酸、奥沙普秦、萘丁美酮、甲酚那酸、酮洛芬等23西药成分用80%甲醇提取,醋酸铵水溶液-甲醇梯度于ACQUITY UPLC BEH C₁₈色谱柱分离,串联四级杆质谱仪检测,MRM方式采集并定量。 结果: 23个药物质谱检测的线性范围宽,相关性好, r²≥0.9901;方法精密度以6次测定值的RSD表示,为2.1% ~ 7.7%; 方法回收率用2个浓度(0.05,1.0 mg·g^-1)进行添加实验,较高浓度时的回收率范围在94.2%~110%;最低定量限(LLOQ)规定为添加回收实验中S/N≥10时的最低添加浓度,23个药物的LLOQ为0.0013~0.05 μg·g^-1。 结论: 本法可用于中成药制剂中多组分解热镇痛药和非甾体抗炎药的同时定量测定。

Objective: To develop a highly selective LC-MS/MS method using a tandem quadrupole mass spectrometer detector for rapidly screening,qualitative identifying and accurate quantifying of 23 nonsteroidal anti-inflammatory (NSAIDs) added in the traditional Chinese medicine preparations. Methods: Acetaminophen,aspirin,metamizole,antipyrine,loxoprofen,antondine,piroxicam,naproxen,sulindac,meloxicam,chlorzoxazone,fenbufen,ibuprofen,diclofenac,indometacin,benorilate,nimesulide,aceclofenac,oxaprozin,nabumetone,mefenamic acid,ketoprofen,celecoxib added in the blank ground samples were extracted with 80% methanol and were separated from a ACQUITY UPLC BEH C₁₈ column within 12 min with a gradient of methanol-ammonium acetate,a tandem quadrupole mass spectrometer equipped with electrospray ionization source (ESI) was used in positive-negative ion mode,multiple reaction monitoring(MRM) was performed to quantify these compounds. Results: 23 linear calibration curves were obtained with r²≥0.9901.The precision of the method were showed as RSD(n =6)ranged from 2.1% to 7.7%.The recoveries were tested at two concentrations (0.05,1.0 mg·g^-1) and ranged from 94.2% to 110% for the higher concentration.The lowest limit of quantification (LLOQ) is defined as the lowest concentration giving the signal-to-noise ≥ 10∶1,the data were 0.0013-0.05 μg·g^-1. Conclusion: The results indicate that the method can be used in quantificational measure of nonsteroidal anti-inflammatory agents on traditional Chinese medicine preparations.

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