液相色谱-串联质谱法同时快速测定婴幼儿配方乳粉中氯丙嗪、醋酸甲孕酮、塞拉嗪、黄曲霉毒素M1和苯甲酸雌二醇残留  

Simultaneous determination of chlorpromazine, medroxyprogesteroneAcetate, xylazine, aflatoxin M1 and estradiol benzoate in infant milk powder by LC-MS/MS

作　　者：王浩[1] 杨红梅[1] 郭启雷[1] 刘艳琴[1] 史海良[1] 田艳玲[1] 

机构地区：[1]国家食品质量安全监督检验中心,北京100094

出　　处：《食品科技》2013年第3期315-318,共4页Food Science and Technology

基　　金：国家质检总局质检公益性行业科研专项(200910267-02)

摘　　要：建立了婴幼儿配方乳粉中氯丙嗪、醋酸甲孕酮、塞拉嗪、黄曲霉毒素M1和苯甲酸雌二醇多残留的高效液相色谱-串联四极杆质谱联用测定方法。样品经碱性乙腈超声提取,以MGⅢ-C18色谱柱(2.1mm×150mm,1.8μm)分离,流动相为10mmol/L乙酸铵水溶液和甲醇(梯度洗脱),流速0.25mL/min。采用多反应监测正离子模式,可以同时对婴幼儿配方乳粉中的氯丙嗪、醋酸甲孕酮、塞拉嗪、黄曲霉毒素M1和苯甲酸雌二醇进行定性和定量测定。方法的检出限为0.3～5.0μg/kg。在5、25、250μg/kg3个加标水平下,加标回收率为76.7%～102.1%,相对标准偏差为1.35%～8.80%。A quick confirmative method was developed for determining the residues of chlorpromazine, medroxyprogesteroneAcetate, xylazine, aflatoxin M1 and estradiol benzoate in infant milk powder by LC- MS/MS. The sample was ultrasonic extracted with alkaline acetonitrile, the HPLC separation was carried out on a MGⅢ-C18 column （2.1 mm×150 mm, 1.8 μm）, the mobile phase were 10 mmol/L ammonium acetate solution and methanol with gradient elution, the flow was 0.25 mL/min. The detection of chlorpromazine, medroxyprogesteroneAcetate, xylazine, aflatoxin M1 and estradiol benzoate were carried out in the positive multi-reaction monitoring （MRM） mode. Under the optimal conditions, good linear relationship were obtained in the range of 1.0-25.0 pg/L for chlorpromazine, medroxyprogesteroneAcetate, xylazine, aflatoxin M1 and estradiol benzoate. The limit of detection were in the range of 0.3-5 IJg/kg. The recoveries at three spiked levels of 5, 25, 250 IJg/kg were between 76.7% and 102.1%, and RSDs value were between 1.35% and 8.80%.

关 键 词：液质联用仪 婴幼儿配方乳粉 氯丙嗪 醋酸甲孕酮 塞拉嗪 黄曲霉毒素M1 苯甲酸雌二醇 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]