植物油中氯丙醇酯和缩水甘油酯质控样品的研制

Development of quality control samples for quantification of chloropropanediol esters and glycidyl esters in vegetable oil

目的研制用于氯丙醇酯和缩水甘油酯含量测定的植物油质控样品。方法以污染水平较高的市售茶油,与不含待测物的空白橄榄油进行混合,制备得到两个浓度水平的质控样品。用气相色谱-质谱法测定氯丙醇酯和缩水甘油酯的含量。均匀性检验用方差分析,质控品的稳定性用t检验评价;组织全国24个实验室参加方法验证的方式进行定值。结果质控样品的均匀性满足要求,室温下储存9个月后3类组分的含量不变,表明稳定性良好。质控样品1的3-氯-1,2-丙二醇酯(3-MCPDE)、2-氯-1,3-丙二醇酯(2-MCPDE)和缩水甘油酯(GE)的定值分别为2.43、1.21、0.672mg/kg;质控样品2的定值分别为1.85、0.841和0.538mg/kg。结论所研制的质控样品性能良好,可用于氯丙醇酯和缩水甘油酯测定的质量控制及测定方法的可靠性验证与评价;本文为油脂类质控品的研制提供了有益的做法。

Objective To develop the quality control samples for determination of chloropropanediol esters(MCPDE)and glycidyl esters(GE)content in vegetable oils.Methods Tea oil with high levels of MCPDE and GE and olive oil sample without analytes were mixed from the local market,getting two quality control(QC)samples.The contents of MCPDE and GE were detected by gas chromatography-mass spectrometry.The evaluation of homogeneity of QC samples was by variance analysis,the evaluation of stability by t test.The assigned values was determined by 24participating laboratory in China.Results The homogeneity and stability of the prepared QC samples met the requirements for method validation or proficiency test,the contents of three components remained unchanged after 9months storage at room temperature.The assigned values of 3-chloro-1,2-propanediol ester(3-MCPDE),2-chloro-1,3-propanediol ester(2-MCPDE)and GE of sample 1were 2.43,1.21,0.672mg/kg,and those of sample 2were 1.85,0.841and 0.538mg/kg,respectively.Conclusion The vegetable oil samples for quality control showed good performance.The developed samples were suitable for quality control,method validation and laboratory proficiency evaluation when quantifying 3-MCPDE,2-MCPDE and GE.This research provides a scientific and valuable method for the development of reference materials or QC samples based on vegetable oil.