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作 者:吕稳 李红英 李丽霞 丁晓萍 Lü Wen;LI Hongying;LI Lixia;DING Xiaoping(Hubei Institute for Drug Control,Wuhan 430075,China;Hubei Engineering Research Center for Drug Quality Control,Wuhan 430075,China)
机构地区:[1]湖北省药品监督检验研究院,武汉430075 [2]湖北省药品质量检测与控制工程技术研究中心,武汉430075
出 处:《理化检验(化学分册)》2021年第5期470-475,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:湖北省食品药品监督管理局资助项目(201801009)。
摘 要:建立了超高效液相色谱-串联质谱法(UHPLC-MS/M S)测定化妆品中21种抗组胺类药物的方法。样品用甲醇提取后,采用Waters ACQUITY UPLC BEH-C 18色谱柱分离21个组分,以甲醇-含0.1mol·L^(-1)甲酸铵的0.1%(体积分数)甲酸溶液为流动相进行梯度洗脱,在电喷雾离子源正离子(ESI+)模式下电离,多反应监测(MRM)模式下检测。结果显示:21种抗组胺类药物的质量浓度均在5~250μg·L^(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为0.1~0.5μg·L^(-1)。在3种基质中的加标回收率为80.2%~110%,测定值的相对标准偏差(n=6)为1.5%~7.9%。方法用于50批面膜样品的分析,均未检出21种抗组胺类药物。A method for the determination of 21antihistamines in cosmetics by UHPLC-MS/MS was established.Samples were extracted with methanol,then 21components were separated on an Waters ACQUITY UPLC BEH-C 18 column with mixed solution composed of methanol and 0.1%(volume fraction)formic acid solution(containing 0.1mol·L^(-1)ammonium formate)as mobile phase for gradient elution.Detection was carried out by ESI+in MRM mode in MS/MS analysis.Linearity relationships between mass concentrations of the 21 antihistamines and their peak areas were kept in the same range of 5-250μg·L-1,with detection limits(3 S/N)in the range of 0.1-0.5μg·L-1.The recoveries on three substrates were found in the range of 80.2%-110%,w ith RSDs(n=6)of determined values ranged from 1.5%to 7.9%.The proposed method was applied for the analysis of 50batches of mask samples,and none of 21antihistamines were found.
关 键 词:超高效液相色谱-串联质谱法 抗组胺类药物 化妆品
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