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    同位素稀释-气相色谱-质谱法测定食品接触纸制品中3-氯-1,2-丙二醇和1,3-二氯-2-丙醇的迁移量

    Determination of Migration Amounts of 3-Chloro-1,2-Propanediol and 1,3-Dichloro-2-Propanol in Food Contact Paper Products by Gas Chromatography-Mass Spectrometry with Isotope Dilution

    • 摘要: 建立了同位素稀释-气相色谱-质谱法(GC-MS)同时测定食品接触纸制品中3-氯-1,2-丙二醇(3-MCPD)和1,3-二氯-2-丙醇(1,3-DCP)迁移量的方法。以4%(体积分数,下同)乙酸溶液、10%(体积分数,下同)乙醇溶液、50%(体积分数,下同)乙醇溶液和橄榄油为食品模拟物,根据GB 5009.156-2016和GB 31604.1-2015对样品进行迁移试验。称取迁移后的样品溶液10.00 g,经5 mL异辛烷(4%乙酸溶液、10%乙醇溶液、50%乙醇溶液)或2 mL甲醇(橄榄油)萃取,离心,氮吹至近干后,再加入含100 μg·L-1 3-MCPD-d5和1,3-DCP-d5的内标溶液1.0 mL,得到样品浓缩液。用气密针向样品浓缩液中加入20 μL衍生试剂含1%(质量分数)三甲基氯硅烷的N,O-双(三甲基硅烷基)三氟乙酰胺溶液,于80℃衍生60 min。采用GC-MS分析,内标法定量。结果显示:3-MCPD、1,3-DCP标准曲线的线性范围均为5~100 μg·L-1,检出限(3s)均为1.0 μg·kg-1;对一次性纸盘子样品进行3个浓度水平的加标回收试验,3-MCPD和1,3-DCP的回收率分别为81.0%~91.2%和82.0%~93.8%,测定值的相对标准偏差(RSD,n=6)分别为3.2%~6.6%和2.6%~6.3%。方法用于测定10种食品接触纸制品中3-MCPD和1,3-DCP的迁移量,其中9种样品中均检出了3-MCPD,3种样品中检出了1,3-DCP。

       

      Abstract: A method for simultaneous determination of migration amounts of 3-chloro-1,2-propanediol (3-MCPD) and 1,3-dichloro-2-propanol (1,3-DCP) in food contact paper products by gas chromatography-mass spectrometry (GC-MS) with isotope dilution was established. 4% (φ, the same below) acetic acid solution, 10% (φ, the same below) ethanol solution, 50% (φ, the same below) ethanol solution and olive oil were used as food simulators, and the migration tests of sample were conducted according to GB 5009.156-2016 and GB 31604.1-2015. The migrated sample solution of 10.00 g was extracted by 5 mL of isooctane (4% acetic acid solution, 10% ethanol solution, 50% ethanol solution) or 2 mL of methanol (olive oil), and the concentrated sample solution was prepared after being centrifuged, blown with nitrogen to nearly dry, and dissolved by 1.0 mL of internal standard solution containing 100 μg·L-1 3-MCPD-d5 and 1,3-DCP-d5. Derivative reagentN,O-bis (trimethylsilalkyl) trifluoroacetamide solution containing 1% (mass fraction) trimethylchlorosilane of 20 μL was added with an airtight needle and the solution was derivatized at 80℃ for 60 min. GC-MS and internal standard method were used for quantitative analysis. As shown by the results, linear ranges of standard curves for 3-MCPD and 1,3-DCP were in the same range of 5-100 μg·L-1, with detection limits (3s) of 1.0 μg·kg-1. Recovery test was made on disposable paper plate sample at 3 concentration levels by standard addition method, giving results of 3-MCPD and 1,3-DCP in the ranges of 81.0%-91.2% and 82.0%-93.8%, and RSDs (n=6) of the determined values ranged from 3.2% to 6.6% and from 2.6% to 6.3%. This method has been applied for determination of migration amounts of 3-MCPD and 1,3-DCP in 10 kinds of food contact paper products. 3-MCPD was detected in 9 samples and 1,3-DCP was detected in 3 samples.

       

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