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本文建立了氧化除杂-气相色谱/质谱联用测定食品中石蜡的检测方法。样品加入环己烷超声浸提2次,离心收集浸提液,加入复配氧化试剂(三氧化铬:浓硫酸:水=1:1:2)氧化除杂,过硅胶小柱净化,气相色谱-质谱联用检测。结果表明:富含油脂的火锅底料样品方法线性范围40~800 mg/kg,相关系数0.9991,最低检测限8 mg/kg;油脂含量低的干香菇、粉条样品方法线性范围10~400mg/kg,相关系数0.9995,最低检测限3.5 mg/kg,加标实验方法平均回收率在90~117%,相对标准偏差在2.7~6.4%。该方法反应温和,未引入干扰检测的副产物,操作简便,通用性强,适用于富含油脂的火锅底料以及油脂含量较低的干香菇、粉条、大米、瓜子等食品。
In this paper, a method for the determination of paraffin in food by oxidative decontamination combined with gas chromatography / mass spectrometry was established. The sample was extracted twice with cyclohexane and centrifuged to collect the extract. The mixture was oxidized and removed by complex oxidation reagent (chromium trioxide: concentrated sulfuric acid: water = 1: 1: 2) and purified by silica gel column chromatography - Mass spectrometry combined detection. The results showed that the linear range of 40 ~ 800 mg / kg, the correlation coefficient of 0.9991, and the lowest detection limit of 8 mg / kg were obtained for the samples of the oil-rich hot pot bottom material. The linear range of the dried mushrooms and vermicelli samples with low fat content was 10 ~ 400 mg / kg , The correlation coefficient was 0.9995, the lowest limit of detection was 3.5 mg / kg. The average recoveries of spiked test methods were 90-117% with relative standard deviations of 2.7-6.4%. The method has the advantages of mild reaction, no by-product of interference detection, simple and convenient operation and strong universality, and is applicable to the oil-fueled pot bottom material and the dried mushrooms, vermicelli, rice and melon seeds and other foods with low fat content.