凉茶中20种抗炎类药物的HPLC-MS同时快速测定法

Simultaneous rapid determination of 20 anti-inflammatory drugs in herbal tea by HPLC-MS

目的 建立高效液相色谱-串联质谱(high-performance liquid chromatography-tandem mass spectrometry,HPLC-MS)方法快速测定凉茶中非法添加的20种抗炎类药物(甲硝唑、磺胺吡啶、磺胺甲恶唑、依诺沙星、氧氟沙星、氟罗沙星、莫西沙星、诺氟沙星、环丙沙星、林可霉素、克林霉素、克林霉素磷酸酯、阿奇霉素、克拉霉素、罗红霉素、氯霉素、螺内酯、灰黄霉素、克霉唑、氟康唑)。方法 采用电喷雾离子源,正/负离子多反应检测,液相色谱-质谱分离,基质曲线外标法定量。结果 20种抗炎药物在2.5~25.0 ng/mL(克林霉素磷酸酯为50~500 ng/mL)的质量浓度范围内线性良好,经过0.5%甲酸化乙腈提取,对阴性样品加标量为0.005 0、0.012 5、0.020 0μg/g范围内的回收率为75%~126%。结论 该方法适应范围广、灵敏度高并且高效,能满足实际样品检测的需要。

Objective To establish amethod of high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS) for the rapid determination of 20 anti-inflammatory drugs illegally added in herbal tea(metronidazole,sulfapyridine,sulfamethoxazole,enoxacin,ofloxacin,fleroxacin,ciprofloxacin,norfloxacin,ciprofloxacin,lincomycin,clindamycin,clindamycin phosphate,azithromycin,clarithromycin,roxithromycin,chloramphenicol,spironolactone,griseofulvin steroids,clotrimazole,fluconazole). Methods The electrospray ion source,positive/negative ion multiple reaction detection,liquid chromatography-mass spectrometry separation,and matrix curve external standard method were used for quantification. Results The 20 anti-inflammatory drugs had good linearity in the mass concentration range of 2.5-25.0 ng/mL(50-500 ng/mL for clindamycin phosphate). After extraction with 0.5% formic acid acetonitrile,the recoveries of the spiked amount of negative samples(0.005 0,0.012 5 and 0.020 0 μg/g) were all 75%-126%.Conclusion The method has wide adaptability,high sensitivity and high efficiency,which can meet the needs of actual sample detection.