食品中脂肪酸氯丙醇酯含量的气相色谱-质谱测定法

Determination of chloropropanol esters in food by gas chromatography and mass spectrometry

目的建立气相色谱-质谱法定量测定食品中脂肪酸氯丙醇酯含量的方法。方法通过样品中脂肪的水解液进行净化,再浓缩和衍生后,经气相色谱-质谱法(GC-MS)测定,以稳定性同位素内标法对3-氯-l,2-丙二醇酯(3-MCPD酯)和2-氯-l,3-丙二醇酯(2-MCPD酯)进行定量。以选择离子扫描(SIM)模式监测目标化合物的特征离子进行定性定量分析。结果建立的方法目标化合物在测定的范围内线性关系良好(r>0.999),方法的检出限为0.027 mg/kg(S/N=3)。在加标水平为0.75、1.00、2.00 mg/kg时,方法的回收率为94.0%~104.0%,相对标准偏差为3.10%~7.20%。结论该方法选择性好,灵敏度高和精密度好,适用于食品中脂肪酸氯丙醇酯含量的测定。

[Objective]To establish a method for the determination of chloropropanol esters in food by gas chromatography and mass spectrometry（GC-MS）. [Method] The hydrolysate of the fat in the samples was purified, and measured by GC-MS after enrichment and derivatization. The stable isotope internal standard method was used to quantitatively measure 3-chloro-l,2-propylene glycol ester（3-MCPD ester） and 2-chloro-l, 3-propylene glycol ester（2-MCPD ester）. The qualitative and quantitative analysis was performed by the monitoring of the characteristic ions of the target compounds with selective ion scanning（SIM）model. [Results] The established method has a good linear relationship in the determination range of target compounds（r〉0.999）,and the detection limit of the method was 0.027 mg/kg（S/N=3）. When the standard addition level was 0.75, 1.00 and 2.00 mg/kg, the recovery rates were 94.0%-104.0%, and the standard deviation was 3.10%-7.20%. [Conclusion] The method has good selectivity, high sensitivity and good precision, which is suitable for the determination of chloropropanol esters in food.