Zhang Jin, Yang Lizhong, Lin Liyi, Chen Luping, Zhou Yu, Xu Dunming
Inspection and Quarantine Technology Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China.
Se Pu. 2011 Jul;29(7):637-42.
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/ MS) method was established for the determination of spinosyns A and D residues in foodstuffs. The food samples were extracted with acetonitrile-water (50:50, v/v), and then purified by an HLB solid phase extraction (SPE) column. The analytes were determined by HPLC-MS/MS and quantified by external standard method. The mass spectrometric detection was operated with electrospray in positive ionization mode and the spinosyns A and D were identified in multiple reaction monitoring (MRM) mode. The linear range of the method was 1-20 microg/L, with the correlation coefficient (r2) of 0.999 9. No significant matrix effect was found for spiked samples. The recoveries of spinosyns A and D spiked in food were 76.2%-114.0% at the spiked levels of 1-10 microg/kg. The relative standard deviations (RSDs) were less than 10%. The limits of detection (LODs) and quantification (LOQs) were 0.2 microg/kg and 0.5 microg/kg for spinosyn A, 0.5 microg/kg and 1.0 microg/kg for spinosyn D, respectively. The proposed procedure was applied to the analysis of 969 real samples from Xiamen, Fujian Province (China), of which 15 positive samples were found. The results showed that the proposed method is sensitive and accurate for the determination of spinosyns A and D in foodstuffs.
建立了一种高效液相色谱-串联质谱（HPLC-MS/MS）法测定食品中多杀菌素A和D的残留量。食品样品用乙腈-水（50:50，v/v）提取，然后通过HLB固相萃取（SPE）柱进行净化。采用HPLC-MS/MS测定分析物，并通过外标法进行定量。质谱检测采用电喷雾正离子模式，在多反应监测（MRM）模式下鉴定多杀菌素A和D。该方法的线性范围为1-20μg/L，相关系数（r2）为0.999 9。加标样品未发现明显基质效应。在1-10μg/kg的加标水平下，食品中多杀菌素A和D的回收率为76.2%-114.0%。相对标准偏差（RSDs）小于10%。多杀菌素A的检测限（LODs）和定量限（LOQs）分别为0.2μg/kg和0.5μg/kg，多杀菌素D的检测限和定量限分别为0.5μg/kg和1.0μg/kg。将该方法应用于福建省厦门市969份实际样品的分析，发现15份阳性样品。结果表明，该方法用于测定食品中多杀菌素A和D灵敏且准确。
