离线SPE-LVI-GC-FID法分析婴儿配方奶粉中的饱和烃类矿物油

发布时间：2018-06-29 20:45

本文选题：婴儿配方奶粉 + 饱和烃类矿物油(MOSH)　；参考：《食品科学》2017年22期

【摘要】：建立婴儿配方奶粉中饱和烃类矿物油(mineral oil saturated hydrocarbons,MOSH)的离线固相萃取(solid phase extraction,SPE)结合大体积进样-气相色谱-氢火焰离子化检测器(large volume injection-gas chromatographyflame ionization detection,LVI-GC-FID)的分析方法。该方法以正己烷为提取溶剂,提取液经硝酸银渍硅胶SPE柱净化;通过比较不同长径比SPE柱的净化效果,确定以5 mL玻璃注射器作为分离MOSH的SPE柱,收集洗脱液5 mL,浓缩后注入LVI-GC-FID测定。GC的进样口升温程序为:初始温度45℃,保持1 min(分流比200∶1),以250℃/min升温至360℃(分流阀关闭2 min),并保持27 min(分流比为100∶1);柱温箱升温程序为:35℃保持3 min,以25℃/min升温至350℃,再以5℃/min升温至370℃,保持10 min;FID温度380℃;进样量40μL。结果表明:MOSH的标准品液体石蜡在2~500 mg/kg范围内呈良好线性关系,相关系数为0.999,方法的定量限为0.05 mg/kg,加标回收率在92.62%~102.86%之间,相对标准偏差在0.85%~2.57%之间,适用于婴儿配方奶粉中MOSH的定量分析。应用该方法检测市售10种婴儿配方奶粉中的MOSH含量,其结果在0.24~1.30 mg/kg之间,其中MOSH(C16~C35)含量在0.12~0.85 mg/kg之间,表明有必要对婴儿配方奶粉中的矿物油污染进行监管。
[Abstract]:An off-line solid phase extraction (solid phase extraction, SPE) of saturated hydrocarbon mineral oil (mineral oil saturated hydrocarbons, MOSH) in infant formula milk powder is established and the analytical method of mass injection gas chromatography hydrogen flame ionization detector (large volume injection-gas) is established. Methods with hexane as extraction solvent, the extraction solution was purified by SPE column with silver nitrate with silica gel. By comparing the purification effect of SPE column with different length and diameter ratio, 5 mL glass syringe was used as SPE column for separating MOSH, and 5 mL of eluent was collected. After concentrated injection LVI-GC-FID, the program of temperature rising of.GC at the initial temperature was 45, 1 min (distributary). Compared with 200: 1), heating up to 360 C at 250 /min (2 min), and maintaining 27 min (the shunt ratio of 100: 1), the temperature box of column temperature kept 3 min at 35 C, heating to 350 centigrade at /min at 35 degrees C, and then to 5 degrees /min to 370 degrees C, FID temperature, and L. results showed that MOSH's standard liquid paraffin wax was in 2~500 mg/kg There is a good linear relationship in the range, the correlation coefficient is 0.999, the method's quantitative limit is 0.05 mg/kg, the recovery rate is 92.62%~102.86%, the relative standard deviation is between 0.85%~2.57% and the quantitative analysis of MOSH in the infant formula milk powder. The method is used to detect the MOSH content in the 10 kinds of infant formula milk powder, and the result is in 0.24~1.3 The content of MOSH (C16~C35) is between 0.12~0.85 mg/kg and 0 mg/kg, indicating that it is necessary to supervise the pollution of mineral oil in infant formula.
【作者单位】：北京市理化分析测试中心北京市食品安全测试工程技术研究中心北京市科学技术研究院分析测试技术重点实验室;国防科技大学西安通信学院;
【基金】：北京市科技计划课题(Z161100000616005) 北京市科学技术研究院财政专项(PXM2016_178305_000013;PXM2017_178305_000001)
【分类号】：O657;TS252.51

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