气相色谱-三重四极杆串联质谱法测定肉制品中7种己二酸酯类物质残留

Determination of 7 kinds of adipate esters residues in meat products by gas chromatography-triple quadrupole tandem mass spectrometry

中文关键词:  气相色谱-三重四极杆串联质谱法  己二酸酯类物质  肉制品

英文关键词:gas chromatography-triple quadrupole tandem mass spectrometry  adipate esters  meat products

中文摘要:

      目的 建立气相色谱-三重四极杆串联质谱法同时测定7种己二酸酯类物质残留量的分析方法, 并对肉制品中7种己二酸酯类物质进行筛查。方法 样品经乙腈提取, 提取液用SinChERS-General柱净化, 多反应监测模式进行检测, 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, 满足定量分析要求。该方法线性关系良好, 7种己二酸酯类物质的线性范围为0.01~0.40 mg/L, 相关系数(r2)均大于0.999。在0.04、0.10、0.20 mg/kg 3个不同加标浓度水平下, 7种己二酸酯类物质的回收率为73.5%~117.5%, 相对标准偏差(relative standard deviations, RSDs)为0.8%~8.2%。方法检出限为0.01 mg/kg, 方法定量限为0.03 mg/kg。对59份肉制品中的7种己二酸酯类物质含量进行检测分析, 结果显示, 有6份样品检出, 其中己二酸二(2-乙基己基)酯的检出浓度为0.071~5.930 mg/kg, 双(1-丁基戊基)己二酸酯的检出浓度为0.056~0.480 mg/kg, 其他己二酸酯类物质均未检出。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7种己二酸酯类物质残留的同时测定。

英文摘要:

      Objective To establish an analytical method for simultaneous determination of 7 kinds of adipate esters residues in meat products by gas chromatography-triple quadrupole tandem mass spectrometry. Methods The samples were extracted with acetonitrile, and the extract was purified by SinChERS-General solid-phase extraction column, detected under multi-reaction 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 analysis requirements. The linear relationship of the method was good. The linear ranges of the 7 kinds of adipate esters were 0.01?0.40 mg/L, and the correlation coefficients (r2) were greater than 0.999. The recoveries of the 7 kinds of adipate esters at the 3 spiked concentrations of 0.04, 0.10, and 0.20 mg/kg were 73.5%?117.5%, and the relative standard deviations (RSDs) were 0.8%?8.2%. The limits of detection were 0.01 mg/kg, and the limits of quantitation were 0.03 mg/kg. The content of 7 kinds of adipate esters in 59 meat products was detected. The results showed that 6 samples were detected, among which the concentration of diethylhexyl adipate was 0.071?5.930 mg/kg, and the concentration of bis(1-butylpentyl) adipate was 0.056?0.480 mg/kg. Other adipate esters were undetected. Conclusion The method has the advantages of simple pretreatment, high sensitivity, high accuracy and strong anti-interference ability, and can simultaneously determine the residue of 7 kinds of adipate esters in meat products.