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目的:建立一种灵敏、快捷的LC-MS/MS方法,快速检测皮肤科常用中药制剂中添加的氯雷他定、盐酸苯海拉明、盐酸赛庚啶、盐酸西替利嗪、盐酸异丙嗪、咪唑斯汀、马来酸氯苯那敏7种抗组胺化学药物。方法:片剂、软膏和洗剂等样品均采用甲醇超声溶解、离心的方法进行前处理。LC-MS/MS条件:采用Agilent Eclipse Plus C_(18)(2.1 mm×50 mm,3.5μm)色谱柱,以含0.1%甲酸的乙腈(A)-含0.1%甲酸的水(B)为流动相,进行梯度洗脱(0~0.1 min,5%A→95%A;0.1~4.1 min,95%A;4.1~8 min,95%A→5%A),流速0.4 mL·min~(-1),柱温40℃;选择ESI正离子模式扫描,信号采集方式为多反应监测(MRM)。最后通过比较MRM通道中样品峰与对照品峰及色谱保留时间等信息确定受试样品是否被添加上述抗组胺药物。结果:在一定浓度范围内,氯雷他定、盐酸苯海拉明、盐酸赛庚啶、盐酸西替利嗪、盐酸异丙嗪、咪唑斯汀和马来酸氯苯那敏7种抗组胺化学药物有较好的线性和稳定性,且检测下限均在0.5~2.5 ng·mL~(-1),定量下限均在1~5 ng·mL~(-1),回收率均在86.2%~112.5%范围内。在9种中药制剂中,4种被检出添加了抗组胺药物。结论:本方法经方法学验证,可作为皮肤科中药制剂中检出添加抗组胺化学药物的检测方法。
OBJECTIVE: To establish a sensitive and rapid LC-MS / MS method for the rapid detection of loratadine, diphenhydramine hydrochloride, cyproheptadine hydrochloride, cetirizine hydrochloride, and hydrochlorothiazide Mesotrazine, mizolastine, chlorpheniramine maleate 7 kinds of antihistamines. Methods: Samples of tablets, ointment and lotion were pretreated by ultrasonic dissolution of methanol and centrifugation. LC-MS / MS conditions: acetonitrile (A) containing 0.1% formic acid - water (B) containing 0.1% formic acid was flowed on an Agilent Eclipse Plus C 18 (2.1 mm x 50 mm, (0 to 0.1 min, 5% A to 95% A; 0.1 to 4.1 min, 95% A; 4.1 to 8 min, 95% A to 5% A) at a flow rate of 0.4 mL · min to -1). The column temperature was 40 ℃. The ESI positive mode was selected and the signal acquisition mode was MRM. Finally, by comparing the MRM channel sample peak with the reference peak and chromatographic retention time and other information to determine whether the test sample is added anti-histamine drugs. Results: In a certain concentration range, loratadine, diphenhydramine hydrochloride, cyproheptadine hydrochloride, cetirizine hydrochloride, promethazine hydrochloride, mizolastine and chlorpheniramine maleate 7 kinds of anti-group The linearity and stability of the amine chemicals were good, and the detection limits were both 0.5-2.5 ng · mL -1, with the lower limits of quantification being 1 ~ 5 ng · mL -1 and the recovery rates were 86.2 % ~ 112.5% range. Of the nine TCM preparations, four were found to have antihistamines added. Conclusion: This method is validated by methodology, and can be used as a detection method of adding antihistamine drugs in dermatological Chinese medicine preparations.