Yi Tinghui, Tang Bobin, Zou Yun, Xi Cunxian, Wang Guomin
Chongqing Agricultural Ecological Environment & Resources Protection Station, Chongqing 401121, China.
Chongqing Entry-Exit Inspection and Quarantine Bureau, Chongqing Engineering Technology Research Center of Import and Export Food Safety, Chongqing 400020, China.
Se Pu. 2017 Jul 8;35(7):677-682. doi: 10.3724/SP.J.1123.2017.03009.
A method for the rapid and simultaneous determination of spirotetramat (BYI08330) and its four metabolites in milk was developed with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with acetonitrile for precipitating proteins, degreased with hexane, and analyzed by UPLC-MS/MS in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Good linear relationships between peak areas and mass concentrations of the analytes were obtained in the range of 0.5-50 μ g/L with correlation coefficients greater than 0.998 (=6). The limits of detection (LODs, =3) and limits of quantification (LOQs, =10) were 0.05-0.30 μ g/L and 0.17-1.00 μ g/L, respectively. The recoveries at the spiked levels of 1.0, 2.0 and 10 μ g/L were in the range of 80.0%-108.8% with relative standard deviations (RSDs) of 4.8%-15.2% (=6). The method is fast, sensitive and accurate, and can be used to simultaneously determine BYI08330 and its four metabolites in milk.
建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS),用于快速同时测定牛奶中的螺虫乙酯(BYI08330)及其四种代谢物。样品用乙腈提取以沉淀蛋白质,用正己烷脱脂,然后采用正电喷雾电离和多反应监测(MRM)模式的UPLC-MS/MS进行分析。在0.5-50μg/L范围内,分析物的峰面积与质量浓度之间具有良好的线性关系,相关系数大于0.998(n=6)。检测限(LOD,n=3)和定量限(LOQ,n=10)分别为0.05-0.30μg/L和0.17-1.00μg/L。在1.0、2.0和10μg/L的加标水平下,回收率在80.0%-108.8%范围内,相对标准偏差(RSD)为4.8%-15.2%(n=6)。该方法快速、灵敏、准确,可用于同时测定牛奶中的BYI08330及其四种代谢物。