摘要
采用顶空提取方式,建立了一种用于乳粉和米粉中残留溶剂的气相色谱检测方法。对顶空平衡温度、平衡时间以及毛细管柱类型和色谱分离条件对结果的影响进行了研究,结果表明：顶空平衡温度为70℃,顶空平衡时间为30 min时,选用DB-624（60 m×0.32 mm×1.80μm）的弹性石英毛细管柱采用程序升温的方法对乙酸乙酯等11种有机溶剂残留能得到很好的分离;该方法采用氢火焰离子化检测器检测,外标法定量。所有组分浓度在0.01-0.5mg/kg范围内有良好的线性关系,相关系数r均大于0.999,平均回收率91.3%-109.4%,相对标准偏差（n=6）2.5%-3.0%,最低检出限为0.014 2-0.048 2 mg/kg。55批次样品检测结果显示：主要残留溶剂为乙酸乙酯和乙酸丁酯,前者浓度略高于后者。危害性较高的苯类溶剂均未检出。该方法快速、准确、灵敏度高,适用于乳粉和米粉中多种溶剂残留量的检测。
A gas chromatography method for the determination of residual solvent in milk powder and ground rice was established with headspace extraction. The influences of the equillqgrium temperalture, equihbrium time and capillary column type and chromatographic separation conditions on the results were investigated. The results showed that 11 kinds of solvent residues like ethyl acetate can be well sepated under the condilion of 70 ℃ of equiliborium temperature, 30 minutes of equilibritwn lime, and fused silica capillary column DB-624 （60 m×0.32 mm× 1.80 μm） by using the method of temperature programming. Use hydrogen flame ionization detector and quantified by external standard method. All species concentrations showed good linear relationship in the range of 0.014）.5 mg/ kg, the linear correlation coefficients were all greater than 0.999, the average recovery ranged fivm 91.3% to 109.4%. The relative standard deviation （n=6） ranged from 2.5% to 3.0%, the detection limit was 0.014 2--0.048 2 mg/kg. The test results of 55 batches of samples showed that： the main residual solvent is ethyl acetate and butyl ~. The concentrations of the former were slightly higher than the latter. The benzene solvents of high criticality were not detected. The method is rapid, accurate, high sensitivity. It is suitable for the detection of a variety of solvent residues in infant milk powder and ground rice.
出处
《食品工业》
北大核心
2015年第2期281-284,共4页
The Food Industry
基金
上海市质量技术监督局公益项目(2012-24)
关键词
顶空-气相色谱
溶剂残留
乳粉
米粉
headspace gas chromatography
solvent residues
milk powder
ground rice
