液相色谱-串联质谱法快速同时测定婴幼儿配方乳粉中氯霉素、三聚氰胺、甲硝唑和洛硝达唑  

Simultaneous Determination of Chloramphenicol,Melamine,Metronidazole,Ronidazole 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：《分析化学》2013年第2期283-287,共5页Chinese Journal of Analytical Chemistry

基　　金：国家质检总局质检公益性行业科研专项(No.200910267-02)资助

摘　　要：建立了婴幼儿配方乳粉中三聚氰胺、氯霉素、甲硝唑和洛硝达唑残留的高效液相色谱-串联四极杆质谱联用测定方法。样品经碱性乙腈提取,以MGⅢ-C18色谱柱(150 mm×2.1 mm,5!m)分离,流动相为60 mmol/L乙酸铵溶液(含0.4‰甲酸)和甲醇,梯度洗脱,流速为0.25 mL/min。采用多反应监测正离子或负离子模式,可以同时对婴幼儿配方乳粉中的三聚氰胺、氯霉素、甲硝唑和洛硝达唑进行快速定性和定量测定。在优化条件下,4种化合物检出限为0.3～50.0!g/kg,方法回收率为61.4%～96.2%,相对标准偏差(RSD)为1.8%～9.8%。采用本方法测定了多种市售婴幼儿配方奶粉。本方法操作简单、测定结果准确,可用于婴幼儿配方奶粉中三聚氰胺、氯霉素、甲硝唑和洛硝达唑残留的同时快速测定。A quick confirmative method was developed for determining the residues of chloramphenicol, melamine, metronidazole and ronidazole in infant milk powder by LC-MS/MS. The sample was extracted with methanol （Including 0.5% formic acid）, the HPLC separation was carried out on a MG 111-C18 column （150 mm×2.1 mm, 5 μm）, the mobile phase was 60 mmol/L ammonium acetate solution （Including 0.4%o formic acid ） and methanol with gradient elution, the flow rate was 0.25 mL/min. The detection of chloramphenicol, melamine, metronidazole and ronidazole was carried out in the positive and negative multi-reaction monitoring （MRM） mode, separately. The limits of detection were 0.3-50.0μg/kg. The overall recoveries varied from 60. 1% to 96.2% , and the relative standard deviations （RSD） were 1. 83% and 9.75 %. The real sample analysis showed that the simple and accurate method can be used for determining the residues of the chloramphenicol, melamine, metronidazole and ronidazole in infant milk powder.

关 键 词：液相色谱-串联质谱 氯霉素 三聚氰胺 甲硝唑 洛硝达唑 乳粉 

分 类 号：O657.63[理学—分析化学]