摘要
目的 建立同时测定食品烘焙用纸包装中9种有机溶剂残留量(丁酮、苯、甲苯、对二甲苯、间二甲苯、邻二甲苯、乙酸乙酯、乙酸丁脂、正丁醇)的方法。方法 通过优化自动顶空(HS)-气相色谱(GC)-串联三重四级杆质谱(MS/MS)仪器的自动顶空进样器、色谱、质谱检测。采用优化条件,样品平衡温度为120 ℃,顶空平衡时间为30 min,用Thermo TG-WAXMS色谱柱分离化合物,进样分流比为25∶1,采用外标法定量,MRM(多反应监测模式)模式GC-MS/MS方式检测食品烘焙用纸。 结果 采用该方法能完全分离9种有机溶剂,且线性良好(相关系数在0.99以上),方法检出限为0.003~0.010 mg/m2,回收率为93.8%~101.5%,RSD范围为1.3%~3.5%。结论 该方法与气相色谱检验方法比较,更简单快捷,分离效果好,结果准确,检出限更低,可用于实际检测大批量食品烘焙用纸包装产品中9种有机溶剂残留量。
Abstract
The work aims to set up a method that can determine 9 kinds of organic solvent residues in food baking paper packaging (butyl ketone, benzene, toluene, terephthalic acid, isophthalic acid, phthalic acid, ethyl acetate, butyl acetate ester, n-butyl alcohol). The headspace sample injector, chromatography and mass spectrometry of automatic headspace (HS)-gas chromatography (GC)-series triple level 4 pole mass spectrometry (MS/MS) were optimized for determination. The optimized conditions were as follows:the sample equilibrium temperature was 120 ℃, the headspace equilibrium time was 30 min, the compounds were separated by Thermo TG-WAXMS chromatographic column, and the injection flow ratio was 25∶1. The quantification was carried out by external standard method and the determination was conducted by GC-MS/MS of MRM mode. 9 kinds of organic solvents could be completely separated, with good linear correlation coefficients of above 0.99, method detection limit between 0.003 ~ 0.010 mg/m2, recovery rate between 93.8% ~ 101.5% and RSD between 1.3% ~ 3.5%. The method is easier and faster compared with gas chromatography, with good separation effect, accurate result and lower detection limit and can be used to actually determine 9 kinds of organic solvent residues in paper packaging products.
周春红, 唐璎, 张志龙, 邓展瑞, 黄佳.
基于HS-GC-MS/MS法测定食品烘焙用纸中9种有机溶剂[J]. 包装工程(技术栏目). 2020(21): 38-44 https://doi.org/10.19554/j.cnki.1001-3563.2020.21.006
ZHOU Chun-hong, TANG Ying, ZHANG Zhi-long, DENG Zhan-rui, HUANG Jia.
Determination of 9 Solvent Residues in Food Baking Paper Packaging by HS-GC-MS/MS Method[J]. Packaging Engineering. 2020(21): 38-44 https://doi.org/10.19554/j.cnki.1001-3563.2020.21.006
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基金
甘肃省质量技术监督局科技项目(SSCJG-ZJ-201907)