High-performance liquid chromatographic method for the determination of cyromazine and melamine residues in milk and pork.
High-performance liquid chromatographic method for the determination of cyromazine and melamine residues in milk and pork.
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DOI：
10.1093/chromsci/47.7.581
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发表时间：
2009-08
影响因子：
1.3
通讯作者：
中科院分区：
文献类型：
--
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本文介绍了一种高效液相色谱法。本方法采用nh2色谱柱和97%乙腈洗脱液测定牛奶和猪肉中杀虫剂氰胺及其代谢物三聚氰胺的残留量。样品用NaOH处理，用含20% NH(4)OH的乙腈提取。样品的目标分析物经C（18）柱固相萃取净化浓缩。氰胺和三聚氰胺分离成功，保留时间分别为8 min和12 min。氰胺和三聚氰胺在0.01 ~ 1.0 μ g/mL范围内均呈良好的线性关系，相关系数分别为0.9999和0.9997。两种化合物的检出限为0.2 ng，定量限为0.02 mg/kg。在强化水平为0.02、0.05和0.1 mg/kg时，氰胺和三聚氰胺的回收率分别为84.5 ~ 90.8%和83.6 ~ 91.3%，变异系数为3.1 ~ 7.8%。
A high-performance liquid chromatography method is described in this paper. The method uses NH(2) column and 97% acetonitrile eluate to determine the insecticide cyromazine and metabolite melamine residues in milk and pork. Samples were treated with NaOH and extracted with acetonitrile containing 20% NH(4)OH. Target analytes of samples were cleaned up and concentrated by C(18) column solid-phase extraction. A separation for cyromazine and melamine was achieved, and respective retention times were 8 and 12 min. The calibration curves for cyromazine and melamine were linear in a concentration range of 0.01-1.0 microg/mL, with correlation coefficients of 0.9999 and 0.9997, respectively. The limit of detection of both compounds was 0.2 ng, and the limit of quantitation was 0.02 mg/kg. Recoveries of cyromazine and melamine at fortified levels of 0.02, 0.05, and 0.1 mg/kg ranged from 84.5-90.8%, and 83.6-91.3%, respectively, with coefficient of variation of 3.1-7.8%.