液相色谱-串联质谱法测定乳粉中氟乙酸钠
目的 基于液相色谱-串联质谱法, 建立衍生化法测定乳粉中氟乙酸钠(1080)的新方法。方法 样品经水-丙酮提取, 阴离子树脂净化后, 由3-硝基苯胺-EDAC衍生和HLB净化处理提取, 通过BEH C18色谱柱进行分离, 电喷雾负离子多反应监测模式进行检测, 内标法定量。结果 氟乙酸钠(1080)在1.0~100.0 ng/mL浓度范围内具有良好的线性, 相关系数r为0.9993, 检出限(limit of detection, LOD)可达到0.3 μg/kg, 不同添加浓度的平均回收率在99.1%~103%之间, 测定结果的相对标准偏差在2.0%~6.2%之间。结论 本方法准确、灵敏度高, 可用于乳粉中氟乙酸钠的快速准确测定和定量分析。
Objective To establish a new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determination sodium fluoroacetate (1080) in milk powder by derivatization treatment. Methods Samples were ultrasonically extracted with water-acetone and purified by anion resin AG 1-X8, and then extracted by 3-nitroaniline-edac derivation and HLB purification treatment. The target compound was separated by BEH C18 (2.1 mm×100 mm, 1.7 μm), and analyzed by a negative electrospray ion multiple reaction monitoring mode. Results Sodium fluoroacetate (1080) had good linear relationships in the range of 1.0?100.0 ng/mL, with correlation coefficients were 0.9993. The limit of detection was 0.3 μg/kg. The recoveries at different spiked levels were 99.1%?103%, with the relative standard deviations (RSDs) of 2.0%?6.2%. Conclusion This method is accurate and sensitive, which can be used in the rapid and accurate determination and quantitative analysis of sodium fluoroacetate in milk powder.
标题：液相色谱-串联质谱法测定乳粉中氟乙酸钠
英文标题：Determination of sodium fluoroacetate in milk powder by liquid chromatography-tandem mass spectrometry
作者：
李克静 中国检验检疫科学研究院综合检测中心
杨秀勇 中国检验检疫科学研究院综合检测中心
赵鑫 中国检验检疫科学研究院综合检测中心
李晓娟 中国检验检疫科学研究院综合检测中心
李淑娟 中国检验检疫科学研究院综合检测中心
中文关键词:氟乙酸钠,液相色谱-串联质谱法,衍生化法,乳粉,
英文关键词:sodium fluoroacetate,liquid chromatography-tandem mass spectrometry,derivatization method,milk powder,
发表日期：2019-06-11
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