Abstract: Objective To analyze the factors influencing the accuracy of determination Results of 3-chloropropane esters in vegetable oil by gas chromatography mass spectrometry so as to put forward effective control measures for acquiring accurate determination results. Methods Gas chromatography-mass spectrometry was used to determine 3-chloropropane esters in vegetable oil samples with pretreatment, including suitable quantitative ion selection, ether purification and adsorbent and dehydrant baking. Results After selecting quantitative ion m/z 453, purifying ether and baking adsorbent and dehydrant under 500℃ for 3 hours, the correlation coefficient of working curve was 0.9995, and the determination values of reagent blank and negative vegetable oil samples were all less than the detection limits. The levels of two parallel determination of 3-chloropropane esters in proficiency testing samples from Food Analysis Performance Assessment Scheme (FAPAS) were both within the acceptable range, and the relative standard deviation (RSD) was 4.6%. Conclusions We find the key factors influencing determination of 3-chloropropane esters in this study. The chromatographic peak area of 3-chloropropane esters can not be integrated accurately when selecting m/z 289 as quantitative ion, but no interference exists using m/z 453. The background of 3-chloropropanol, which exists in ether, adsorbent and dehydrant, can affect the determination of 3-chloropropane esters in vegetable oil samples,so it must be purified.
[1]陈雪桥, 张明霞, 周建科. 气相色谱法测定饼干类食品中氯丙醇类化合物[J]. 分析试验室, 2006, 25(9):57-59. [2] Hrncirik K, Duijn GV. An initial study on the formation of 3-MCPD esters during oil refining[J]. Eur J Lipid Sci Tech,2011,113(3):374-379. [3] 傅武胜, 严小波, 吕华东, 等. 气相色谱/质谱法测定植物油中脂肪酸氯丙醇酯[J]. 分析化学, 2012, 40(9):1329-1335. [4] Chung HY, Chung SW, Chan BT, et al. Dietary exposure of Hong Kong adults to fatty acid esters of 3-monochloropropane-1,2-diol[J]. Food Addit Contam Part A Chem Anal Control Expo Risk Assess, 2013, 30(9):1508-1512. [5] 韩枫, 刘卿, 谢科, 等. 同位素稀释-气相色谱-质谱法测定面包中3-氯-1,2-丙二醇脂肪酸酯[J]. 中国科学:化学, 2014,44(3):389-394. [6] 李珊, 苗虹, 崔霞, 等. 乳粉中氯丙醇脂肪酸酯的气相色谱-质谱检测方法的建立及其污染水平分析[J]. 中华预防医学杂志, 2015, 49(6):554-559. [7] 边天斌, 任韧, 何华丽, 等. 固相萃取气相色谱-质谱法测定杭州市食用植物油中氯丙醇脂肪酸酯[J]. 中国卫生检验杂志, 2016, 26(21):3093-3097. [8] Seefelder W, Varga N, Studer A, et al. Esters of 3-chloro-1,2-propanediol (3-MCPD) in vegetable oils:significance in the formation of 3-MCPD[J]. Food Addit Contam Part A Chem Anal Control Expo Risk Assess, 2008, 25(4):391-400. [9] Joint FAO/WHO Expert Committee on Food Additives. Evaluation of certain food additives and contaminants[J].World Health Organ Tech Rep Ser, 2007(947):1-225. [10] Hwang M, Yoon E, Kim J, et al.Toxicity value for 3-monochloropropane-1,2-diol using a benchmark dose methodology[J]. Regul Toxicol Pharmacol, 2009, 53(2):102-106. [11] Küsters M, Bimber U, Reeser S, et al. Simultaneous determination and differentiation of glycidyl esters and 3-monochloropropane-1,2-diol ( MCPD) esters in different foodstuffs by GC-MS[J]. J Agric Food Chem, 2011, 59(11):6263-6270. [12] 黄剑锋, 吴秀登, 傅武胜. 氯丙醇的安全毒理学评价概况[J]. 实用预防医学, 2002, 9(4):427-430.