影响SPE-GC/MS法检测发酵食品中氨基甲酸乙酯因素的研究

Study on key parameters affecting determination of ethyl carbamate in traditional fermented foods by SPE-GC/MS

CtNSPE—GC／MS法测定Ec的主要影响因素，对萃取小柱类型、型号、洗脱剂用量及检测样品pH等萃取条件进行了优化。结果表明，采用氨基甲酸丙酯（Pc）为内标和选择离子监控模式（SIM），在30～500μg/L范围内具有满意的线性度（R2=0．9992）；常用的4种不同类型的萃取小柱中，硅藻土小柱的通用性较强；15mL二氯甲烷是最佳的洗脱剂用量；检测样品的pH调至7．0后，改善了检测的精度和准确度。优化后的方法在用于基质形态和性质不同样品验证实验的结果显示，该法具有准确度高和抗干扰能力强的特点，且所检测样品的RsD均在5％以下。

In the current study, based on the main factors during EC determination by SPE-GC/MS method,SPE categories and types,elution solvents volume and pH were optimized. The results indicated that good linearity was obtained with a correlation coefficient over 0.9992 ranging from 30 to 500μg/L,using PC as internal standard and SIM mode. By comparing the efficiency of 4 kinds of SPE common used columns,diatomaceous earth column showed satisfactory results. 15mL of elution solvents was optimum elution volume,and precise and accurate results were improved by adjusting of sample solutions to pH7.0. It was shown that the optimized method is more suitable to determine EC accurately and precisely in various types of fermented foods by the validation test for 27 samples of different characteristics and properties,and RSD of EC contents of all samples detected was all below 5%.