全自动固相萃取-UPLC-MS/MS法检测清咽类保健食品中非法添加的盐酸二氧丙嗪和沙丁胺醇  

Determination of Promethazine Hydrochloride and Salbutamol Illegally Added in Qingyan Health Food by Automatic Solid Phase Extraction UPLC-MS/MS

作　　者：王任 吴鸳鸯 胡磊 张丽媛 程巧鸳 WANG Ren;WU Yuanyang;HU Lei;ZHANG Liyuan;CHENG Qiaoyuan(Zhejiang Institute for Food and Drug Control,Hangzhou 310052,China)

机构地区：[1]浙江省食品药品检验研究院,浙江杭州310052

出　　处：《食品工业科技》2021年第16期271-278,共8页Science and Technology of Food Industry

摘　　要：建立全自动固相萃取-超高效液相色谱-串联质谱法(UPLC-MS/MS)检测清咽类保健食品中非法添加的盐酸二氧丙嗪和沙丁胺醇的方法。样品用乙酸铵缓冲溶液和甲醇溶解,采用MCX固相萃取柱进行在线净化,然后通过ACQUITY UPLC BEH C_(18)(2.1 mm×50 mm,1.7μm)分离,以甲酸溶液(0.1%甲酸和10 mmol/L甲酸铵)和甲醇为流动相,梯度洗脱,流速0.2 mL/min,采用电喷雾离子源(ESI)正离子模式,多反应监测(MRM)进行检测。所测盐酸二氧丙嗪和沙丁胺醇的线性范围分别为4.9~49.2 ng·mL^(−1)和4.3~42.7 ng·mL^(−1),线性回归方程的决定系数分别为0.9999和0.9998。盐酸二氧丙嗪和沙丁胺醇呈良好的线性关系,且得到较好的分离度。低、中、高3个添加水平的平均回收率为87.4%~98.8%,RSD为0.83%~3.9%(n=3),盐酸二氧丙嗪和沙丁胺醇的检出下限分别为0.65和0.58μg/kg。经方法学验证,所建立的分析方法可靠、灵敏、准确,可用于清咽类保健食品中非法添加的盐酸二氧丙嗪和沙丁胺醇同时定性和定量分析。A method using UPLC-MS/MS for simultaneous determination of promethazine hydrochloride and salbutamol with automated solid phase extraction in Qingyan health food was established.Samples were extracted by ammonium acetate buffer solution and methanol,then purified by McX solid phase extraction column.The analysis was carried out on ACQUITY UPLC BEH C_(18)(2.1 mm×50 mm,1.7μm)column with isocratic elution using a mobile phase making up of 0.1%aqueous formic acid(10 mmol/L ammonium formate)and methanol at 0.2 mL/min.Mass spectrometry acquisition was done in the positive ion mode and analytes were detected in the MRM mode.The pomethazine hdrochloride and salbutamol linear ranges were 4.9~49.2 and 4.3~42.7 ng·mL^(−1),respectively.Coefficient of determination of linear regression equation of salbutamol and pomethazine hdrochloride were 0.9999 and 0.9998,respectively.Pomethazine hdrochloride and salbutamol could be separately well and had a good linear relationship.The average recovery rates of low,medium and high concentration were 87.4%~98.8%.Relative standard deviation(RSD)was 0.83%~3.9%.The detection limit of promethazine hydrochloride and salbutamol was 0.65 and 0.58μg/kg,respectively.The developed method verified by the methodology was precise,sensitive,accurate,which therefore could be applied for the analysis in Qingyan health food.

关 键 词：沙丁胺醇 盐酸二氧丙嗪 保健食品 全自动固相萃取 超高效液相色谱-质谱联用法 

分 类 号：TS207.2[轻工技术与工程—食品科学]