HPLC-DAD-MS/MS法用于止咳平喘类中成药中添加14种肾上腺皮质激素的筛查和定量研究  

Application of HPLC-DAD-MS/MS to the screening and quantification of 14 adrenocortical hormones adulterated in Chinese patent drugs

作　　者：高辉 李冰 王杰 

机构地区：[1]山东省食品药品检验研究院,济南250101

出　　处：《药物分析杂志》2015年第8期1458-1465,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的：建立HPLC—DAD—MS／MS法用于止咳平喘类中成药中非法添加14种肾上腺皮质激素的筛查和测定。方法：采用VenilsilMPC18（4．6mill×250min,5ulm）色谱柱，以乙腈-甲醇（1：1）及0．3％甲酸铵溶液系统为流动相，梯度洗脱，二极管阵列检测器，检测波长240nln，参比波长360nm，波长扫描范围190—400nm，柱温30℃；质谱装配电喷雾电离源，扫描方式为正、负离子同时进行一级质谱、二级质谱全扫描，扫描范围m／z50～600。干燥气温度325℃，干燥气流速5L·min-1；雾化压力0．1MPa。结果：曲安西龙、地塞米松磷酸钠、泼尼松、氢化可的松、地塞米松、曲安奈德、醋酸泼尼松龙、醋酸氢化可的松、醋酸泼尼松、醋酸可的松、丁酸氢化可的松、醋酸氟轻松、丙酸氯倍他索、丙酸倍氯米松14种肾上腺皮质激素质谱检测限小于1．3μg·mL-1。14种。肾上腺皮质激素加样回收率86．5％．119．1％；在0．42—39．2μg·mL。范围内，线性关系良好（相关系数大于0．999）；4批中成药中检出含醋酸泼尼松。结论：本法经方法学验证，可用于14种肾上腺皮质激素的筛选及确证。Objective：To establish an HPLC-DAD-MS/MS method for simultaneous determination of fourteen adrenocortical hormones adulterated in Chinese patent drugs. Methods：The analysis was performed on a Venusil MP Cis column（4.6 mm × 250 mm,5 μm）with a gradient elution, and the mobile phase was acetonitrile-methanol （1：1） and 0. 3 % formic acid solution. The diode array detector was adopted, the detection wavelength was 240 nm, the reference wavelength was 360 nm,and the scanning range was from 190 to 400 nm. The column temperature was controlled at 30 ℃. The target compounds were analyzed with LC-MS/MS-ESI in two scan modes including full scan MS and full scan MS2. The scan range was m/z 50-600. The drying gas temperature was 325 ℃,the drying gas flow rate was 5 L . min - 1, and the drying gas pressure was 0. 1 MPa. Results： The LOD of mass spectrometric detection limit of fourteen adrenocortical hormones including fluoxyprednisolone, dexamethasone sodium phosphate, metacor- tandracin, hydrocortisone, dexamethasone, fluoxyprednisolone acetonide, prednisolone acetate, hydrocortisone acetate, metacortandracin acetate, cortisone acetate, hydrocortisone butyrate, fluocinonide, clobetasol propionate, beclomethasone were all less than low 1.3 μg . mL-1. The recoveries of fourteen adrenocortical hormones ranged from 86.5 % to 119. 1%. There were good linearities in the range of 0.42 - 39.2 μg .mL- 1 （ r 〉 0. 999 ）. Metacortandracin acetate was found in four batches of counterfeit drugs. Conclusion： The established method has been vali- dated for screening and confirmation of 14 kinds of adrenocortical hormone.

关 键 词：中成药非法添加 曲安西龙 地塞米松磷酸钠 泼尼松 氢化可的松 地塞米松 曲安奈德 醋酸泼尼松龙 醋酸氢化可的 松 醋酸泼尼松 醋酸可的松 丁酸氢化可的松 醋酸氟轻松 丙酸氯倍他索 丙酸倍氯米松 液相色谱-质谱 

分 类 号：R917[医药卫生—药物分析学]