[关键词]
[摘要]
该研究基于分散固相萃取-气相色谱-三重四级杆串联质谱法建立了检测肉制品中15种有机磷酸酯的分析方法。试样中有机磷酸酯经乙腈提取,增强型基质去除吸附剂EMR-Lipid净化,HP-5MS色谱柱分离,采用GC-MS/MS动态多反应离子监测模式进行测定,基质匹配外标法定量。研究结果表明,15种有机磷酸酯的目标化合物在21 min内即可完成色谱分离和分析,并且目标物在0.01~100 ng/mL范围内线性关系良好,相关系数均大于0.999。在1.25、12.5、25 ng/g 3个不同质量浓度加标水平下的15种有机磷酸酯平均加标回收率为72.8%~123.8%,相对标准偏差(n=6)为1.6%~14.7%。方法检出限为0.25~0.40 ng/g,定量限为0.80~1.25 ng/g。将该方法应用到市售的70份肉制品样品中,结果显示,58份样品检测到7种有机磷酸酯,检出率82.8%,其中检出率较高的三种有机磷酸酯分别为磷酸三(2-氯-1-(氯甲基)乙基)酯、磷酸三(2-氯乙基)酯和磷酸三苯酯。该研究建立的方法具备操作简单、快速、净化效果好等优势,可用于肉制品中15种有机磷酸酯的快速检测。
[Key word]
[Abstract]
In this study, an analytical method for the determination of 15 organophosphate esters (OPEs) in meat products was established based on dispersive solid phase extraction-gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). The organophosphates in the sample was extracted with acetonitrile, purified with enhanced matrix removal adsorbent (enhanced matrix removal-lipid, EMR-Lipid), separated by HP-5MS column, determined by GC-MS/MS dynamic multi-reaction ion monitoring (dMRM) mode, and quantified by the matrix matching external standard method. The results showed that chromatographic separation and analysis of 15 OPEs were completed within 21 min, and good linear relationship of the target substances was obtained in the range of 0.01~100 ng/mL, with the correlation coefficients greater than 0.999. The average spike recoveries of 15 kinds of organic phosphate esters at different spiking levels (1.25, 12.5 and 25 ng/g) were 72.8%~123.8%, with the relative standard deviations (RSDs) (n=6) being1.6%~14.7%, the detection limit (LOD) of the method being 0.25~0.40 ng/g and the limit of quantification (LOQ) being 0.80~1.25 ng/g. The method was applied to 70 commercial meat products samples. The results showed that 7 organophosphate esters were detected in 58 samples with a detection rate of 82.8%. Among which, the three organophosphate esters with higher detection rates were tri (2-chloro-1-(chloromethyl) ethyl) phosphate, tri (2-chloro-ethyl) phosphate and triphenyl phosphate. The method established in this study has the advantages of simple operation, high speed and good purification effect, and can be used for the rapid detection of 15 organophosphate esters in meat products.
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[基金项目]
国家市场监督管理总局科技计划项目(SDSJKJ202309);山东省药品监督管理局科研项目(SDNMPAFZLS202301)