气相色谱-质谱法同时测定婴儿配方奶粉和食用植物油中的2-和3-MCPD酯

Huan Yao, Siqi Zeng, Xianghua Wang, Hang Li, Bing Du
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摘要

2-和3-一氯丙烷-1,2-二醇酯(MCPD)是用于食品或食品配料的加工食用油的重要污染物。建立了同时测定婴幼儿奶粉和食用植物油中2 - mcpd酯和3-MCPD酯的气相色谱-质谱联用方法。制定的方案包括婴儿奶粉中的脂肪部分,食用植物油样品提取后用甲基甲醇钠裂解2-和3-MCPD酯的酯键,并以氘同位素标记的2-和3-MCPD棕榈酸双酯和硬脂酸双酯标准样品作为内标。将该方法应用于食品中,具有良好的准确度(MCPD酯的回收率为86% ~ 114%)、较高的灵敏度(3-MCPD和2-MCPD酯的LOD分别为0.025和0.020 mg/kg, LOQ分别为0.075、0.060 mg/kg)和良好的重复性(RSD < 6.8%)。在150份商业食用植物油和婴儿配方奶粉样品中,我们获得了MCPD酯污染的初步概况。
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Simultaneous Determination of 2- and 3-MCPD Esters in Infant Formula Milk Powder and Edible Vegetable Oils by Gas Chromatography-Mass Spectrometry
Esters of 2- and 3-monochloropropane-1,2-diol (MCPD) are significative contaminants of processed edible oils used as foods or food ingredients. The aim of this study was to develop and validate a new method by GC-MS for the simultaneous quantification of 2 and 3-MCPD esters in infant milk powder and edible vegetable oils. The developed protocol included fat fraction in infant milk powder and edible vegetable oils samples was extracted and treated with sodium methylate-methanol to cleave the ester bonds of the 2- and 3-MCPD esters, moreover, standard samples of deuterium isotope-labeled 2- and 3-MCPD palmitic acid double esters and stearic acid double esters were used as the internal standards. Furthermore, this method was validated when it was applied to food products, concrete manifestation in its good accuracy (the recovery of MCPD esters ranged from 86% to 114%), high sensitivity (the LOD of 3-MCPD and 2-MCPD esters were 0.025 and 0.020 mg/kg, LOQ were 0.075, 0.060 mg/kg, respectively) and satisfactory repeatability (RSD below 6.8%) for all analytes. In the 150 commercial edible vegetable oils and infant formula milk powder samples, we obtained a preliminary profile of MCPD ester contamination.
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