QuEChERS结合高效液相色谱串联质谱法测定畜禽肉中工业松香残留

Determination of Industrial Rosin Residues in Livestock and PoultryMeat by QuEChERS Combined with High Performance LiquidChromatography-Tandem Mass Spectrometry

采用QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)结合高效液相色谱串联质谱法建立一种快速检测畜禽肉中工业松香残留的方法。样品中的松香酸和脱氢松香酸2种工业松香残留标志物用乙腈提取,经含PSA、C18、硫酸镁的QuEChERS净化包净化,采用高效液相色谱串联质谱仪进行检测。在0~200 ng/mL浓度范围内,线性关系良好,松香酸和脱氢松香酸的相关系数(R)均达到0.999以上,检出限分别为1.8、4.5μg/kg,定量限分别为3.2、10.6μg/kg,回收率为85.1%~92.1%,相对标准偏差为6.6%~9.7%。模拟工业松香和松香甘油酯脱毛,畜禽肉的表皮和肌肉组织中均有一定量的松香酸和脱氢松香酸检出。变质畜禽表皮组织中由于产生有机胺类物质,使得松香酸和脱氢松香酸回收率降低。试验方法操作简单、灵敏度高,能够快速处理样品,可用于实际样品中工业松香残留标志物的检测分析。

A method for rapid detection of industrial rosin in livestock and poultry meat was established by QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Using acetonitrile extract packet to extracted with two industrial rosin residues,rosin acid and dehydrorosin acid,purified using a QuEChERS purification kit containing PSA,C18 and magnesium sulfate,and analyzed and separated by HPLC-MS/MS.In the linear concentration range of 0–200 ng/mL,the correlation coefficients(R)of rosin acid and dehydrorosin acid were all above 0.999,the detection limits were 1.8 and 4.5μg/kg,and the quantitative limits were 3.2μg/kg and 10.6μg/kg.The recovery rate and relative standard deviation were between 85.1%and 92.1%,and the relative standard deviation were between 6.6%and 9.7%.Simulated depilation of industrial rosin and rosin glyceride showed that a certain amount of abietic acid and dehydroabietic acid were detected in the epidermis and muscle tissue of livestock and poultry meat.The recovery rate of abietic acid and dehydroabietic acid decreased due to the production of organic amines substances in the epidermis tissue of deteriorated livestock and poultry.This method is simple and sensitive,and can be used to detect and analyze industrial rosin residue markers in actual samples.