气相色谱-质谱法同时测定肉制品中6种新型柠檬酸酯类物质残留

Simultaneous determination of 6 kinds of new citrate esters residues in meat products by gas chromatography-mass spectrometry

目的建立气相色谱-质谱法同时测定肉制品中6种新型柠檬酸酯类物质残留量的分析方法。方法样品经乙腈提取,提取液用乙二胺-N-丙基硅烷(primary secondary amine,PSA)/硅胶(silica)复合固相萃取柱净化,选择离子监测(selected ion monitoring,SIM)模式进行检测,基质匹配曲线外标法定量。结果采用基质匹配标准曲线定量的方法降低了基质效应,满足定量要求。该方法线性关系良好,6种柠檬酸酯类物质的线性范围为0.05~2.00 mg/L,相关系数(r~2)均大于0.999。在0.1、0.2、0.5 mg/kg 3个不同加标浓度水平下6种柠檬酸酯类物质的回收率为93.0%~115.3%,相对标准偏差(relative standard deviations,RSDs)(n=6)为1.3%~9.4%。方法检出限为0.01~0.02mg/kg,方法定量限为0.03~0.05mg/kg。结论该方法前处理操作简便,灵敏度高、准确度高、抗干扰能力强,实现了肉制品中6种新型柠檬酸酯类物质残留的同时测定。

Objective To establish an analytical method for simultaneous determination of 6 kinds of new citrate esters residues in meat products by gas chromatography-mass spectrometry. Methods The samples were extracted with acetonitrile, and the extract was purified using a primary secondary amine(PSA)/silica gel composite solid-phase extraction column, detected under selected ion monitoring mode, and quantified by the matrix matching curve external standard method. Results The matrix effect was reduced by the matrix matching standard curve quantification method, which met the quantitative requirements. The linear relationship of the method was good. The linear ranges of the 6 kinds of citrate esters were 0.05-2.00 mg/L, and the correlation coefficients(r~2) were greater than 0.999. The recoveries of the 6 kinds of citrate esters at the 3 spiked concentrations of 0.1, 0.2, and 0.5 mg/kg were 93.0%–115.3%, and the relative standard deviations(RSDs)(n=6) were 1.3%-9.4%. The limits of detection were 0.01-0.02 mg/kg, and the limits of quantitation were 0.03-0.05 mg/kg. Conclusion The method has the advantages of simple pretreatment, high sensitivity, high accuracy and strong anti-interference ability, and can simultaneously determine the residues of 6 kinds of citrate esters in meat products.