Guo Haixia, Xiao Guiying, Zhang Xiqing, Wang Minglin, Li Li, Leng Lei, Gao Hongliang
Se Pu. 2015 Dec;33(12):1242-50. doi: 10.3724/sp.j.1123.2015.09016.
A method has been developed for the simultaneous determination of the 10 kinds of 121 veterinary drugs (including chloramphenicols, β-agonists, sulfonamides, 4-quinolones, nitroimidazoles, macrolides, avermections, polyether antibiotics, tetracycline antibiotics, cephalosporins, etc.) in pork using QuEChERS method coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The drugs were extracted with Na2EDTA-McIlvaine buffer solution (pH = 4) and acetonitrile. Anhydrous sodium sulfate was used for the salting-out process. The solutions divided into two groups were cleaned-up by different mixed sorbents. The drugs were analyzed by UPLC-MS/MS in multiple reaction monitoring (MRM) mode via electrospray ionization. Among the 121 drugs, 5 drugs were quantified by internal standard method, and the other 116 drugs were quantified by external standard method. The calibration curves of the 121 drugs were linear in the range of 0.02-40 μg/L with the correlation coefficients more than 0.99. The limits of quantification (LOQs, S/N = 10) were 0.05-10 μg/kg. The average recoveries of 8 drugs at LOQ level in pork ranged from 41.7% to 59.6% with the relative standard deviations (RSDs) of 1.7% - 13.5%. The average recoveries of 10 drugs at LOQ level in pork ranged from 122.6% to 163.2% with the RSDs of 0.6% -14.8%. The average recoveries of 103 drugs at LOQ level in pork ranged from 60.3% to 118.3% with the RSDs of 0.4% - 16.7%. The proposed method is rapid, simple, sensitive, reliable and cost-effective.
已开发出一种方法,采用QuEChERS方法结合超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定猪肉中121种10类兽药(包括氯霉素类、β-激动剂类、磺胺类、4-喹诺酮类、硝基咪唑类、大环内酯类、阿维菌素类、聚醚类抗生素、四环素类抗生素、头孢菌素类等)。这些药物用Na2EDTA-麦基尔维恩缓冲溶液(pH = 4)和乙腈进行提取。用无水硫酸钠进行盐析过程。分成两组的溶液用不同的混合吸附剂进行净化。通过电喷雾电离在多反应监测(MRM)模式下用UPLC-MS/MS对药物进行分析。在这121种药物中,5种药物采用内标法进行定量,另外116种药物采用外标法进行定量。121种药物的校准曲线在0.02 - 40 μg/L范围内呈线性,相关系数大于0.99。定量限(LOQs,S/N = 10)为0.05 - 10 μg/kg。猪肉中8种药物在定量限水平的平均回收率为41.7%至59.6%,相对标准偏差(RSDs)为1.7% - 13.5%。猪肉中10种药物在定量限水平的平均回收率为122.6%至163.2%,RSDs为0.6% - 14.8%。猪肉中103种药物在定量限水平的平均回收率为60.3%至118.3%,RSDs为0.4% - 16.7%。所提出的方法快速、简单、灵敏、可靠且具有成本效益。