固相萃取与气相色谱⁃质谱法联用测定食用植物油和含脂肪食品中氯丙醇酯的方法验证研究

Method Validation Research for the Determination of Chloropropanol Esters in Edible Vegetable Oil and Fatty Food by Solid‑phase Extraction and Gas Chromatography‑mass Spectrometry

氯丙醇酯是国际上广泛关注的食品加工过程污染物,其水解产物氯丙醇对人体(特别是婴幼儿)危害风险较大。采用固相萃取与气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)联用技术,对食用植物油和含脂食品中的氯丙醇酯[3-氯-1,2-丙二醇脂肪酸酯(简称3-MCPD酯)和2-氯-1,3-丙二醇脂肪酸酯(简称2-MCPD酯)]进行检测。该方法准确度高(3-MCPD酯和2-MCPD酯的平均回收率分别为98.9%和96.5%)、灵敏度高(3-MCPD酯和2-MCPD酯的检出限分别为0.042 mg·kg^(-1)和0.058 mg·kg^(-1))、重现性好(相对标准偏差均低于5%)。76批次监测样品中,3-MCPD酯和2-MCPD酯的含量分别为0.042~4.865 mg·kg^(-1)(平均值为0.773 mg·kg^(-1))和0.058~2.592 mg·kg^(-1)(平均值为0.469 mg·kg^(-1))。经机构间的协同验证和英国FAPAS样的能力验证,2种氯丙醇酯在0.200~3.000 mg·kg^(-1)范围内线性良好,为进一步研究奠定了基础,同时也为食品加工企业严格控制生产过程建立了一种可行的检测方法。

The chloropropanol esters were internationally concerned as pollutants in food processing,its hydrolysates(chloropropanols)has a great risk of harm to human body(especially infants).Therefore,the solid-phase extraction and gas chromatography-mass spectrometry(GC-MS)was used to determining 3-monochloropropane-1,2-diol ester(3-MCPD ester)and 2-monochloropropane-1,3-diol ester(2-MCPD ester)in edible vegetable oil and fatty food.The method had good accuracy(the average recoveries of 3-MCPD ester and 2-MCPD ester were 98.9%and 96.5%,respectively)and sensitivity(the detection limits for 3-MCPD ester and 2-MCPD ester were 0.042 and 0.058 mg·kg^(-1),respectively).Repeatability and reproducibility were satisfactory(the relative standard deviation was below 5%)for all analytes.The concentration of 3-MCPD ester and 2-MCPD ester in 76 batches of monitored samples were in the range of 0.042~4.865 mg·kg^(-1)(the average was 0.773 mg·kg^(-1))and 0.058~2.592 mg·kg^(-1)(the average was 0.469 mg·kg^(-1))respectively.Verified by institutions co-verification and proficiency testing of Food Analysis Performance Assessment Scheme(FAPAS)samples,the two chloropropanol esters showed good linearity in the range of 0.200~3.000 mg·kg^(-1).The results layed a foundation for further research and established a feasible detection method for food processing enterprises to control the manufacturing process strictly.