食品接触材料中9种有机锡的检测
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北京市财政资金项目(PXM2019_178305_000009);北京市改革与发展专项项目(2019ZL0102)。


Determination of 9 Organotins in Food Contact Materials
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Beijing Financial Fund Project (PXM2019_178305_000009); Beijing Reform and Development Project (2019ZL0102).

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    摘要:

    建立了一种同时测定不同用途食品接触材料中有机锡的气相色谱-质谱联用分析方法,对衍生化条件和检测条件进行了优化,在现行标准SN/T 3938—2014《食品接触材料 高分子材料 有机锡的测定 气相色谱-质谱法》检测4种有机锡(二丁基二氯化锡、三丁基氯化锡、二辛基二氯化锡、三苯基氯化锡)的基础上增加至9种(新增:单丁基三氯化锡、三丁基氧化锡、乙辛基三氯化锡、四丁基锡、三环己基氯化锡),并进行了方法学验证实验。该方法在质量浓度为10~2000μg/L线性关系良好,线性相关系数为0.9993~0.9995;方法检出限与定量限分别为5~20μg/kg和15~71μg/kg;方法进样精密度为1.07%~1.82%;中间精密度良好,不同时间、不同实验人员测定结果的RSD值为1.52%~2.65%;方法耐用性测定结果的RSD值为1.51%~2.22%。研究选择了4种市售不同用途的食品接触材料,这些样品为聚氯乙烯材质或含有聚氯乙烯的塑料,如保鲜膜、保温袋内膜、餐垫、饺子冰箱收纳盒等作为研究对象,应用该方法进行检测,检测结果显示这4种食品接触材料中均不含有待测的9种有机锡成分;加标回收率和重复性良好,加标回收率为85.93%~117.39%,对应的RSD值为1.12%~1.97%。此方法灵敏度高、操作简便、结果可靠、通用性强,可用于食品接触材料中9种有机锡的同时检测。

    Abstract:

    An analytical method for simultaneous determination of organotins in food contact materials with different uses by gas chromatography-mass spectrometry was established. The derivatization conditions and detection conditions were optimized and the detection types of organotins were also extended. On the basis of 4 kinds of organtins detection (dibutyltin dichloride, tributyltin chloride, dioctyltin dichloride and triphenyltin chloride) of the current standard of SN/T 3938—2014 “food contact materials-polymers-determination of the organotin compounds-gas chromatography-mass spectrometry”, the detection types of organotins increased to 9 kinds (added:monobutyltin trichloride, tributyltin oxide, mono-n-octyltin trichloride, tetrabutyltin and tricyclohexyltin chloride), and the methodology validation experiments were completed. The good linear relationships were obtained with correlation coefficients of 0.9993-0.9995 in the range of 10-2000μg/L. The limits of detection and quantitation were 5-20μg/kg and 15-71μg/kg, respectively. The injection precisions were 1.07%-1.82%. The intermediate precisions were good, and the relative standard deviation (RSD) of the results detected by different laboratory technicians in different times were 1.52%-2.65%. The RSD of the detection results of durability were 1.51%-2.22%. In this study, 4 kinds of food contact materials with different uses were bought from the market and detected. These samples were made of PVC or plastic containing PVC, such as plastic wrap, heat preservation bag lining, place mat, and refrigerator storage box for dumplings, etc. The results showed that no organotins were detected in these 4 kinds of food contact materials. The recoveries and repeatability were good, the recoveries were 85.93%-117.39%, and the corresponding RSD were 1.12%-1.97%. The established method was highly sensitive, simple, reliable, and versatile, which could be applicable for the simultaneous detection of 9 kinds of organotins in food contact materials.

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钱冲,张梅,勾新磊,白云,刘伟丽,高峡,胡光辉.食品接触材料中9种有机锡的检测[J].食品科学技术学报,2021,39(4):163-170.

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  • 收稿日期:2020-05-18
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  • 在线发布日期: 2021-09-07
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