建立了 QuEChERS结合超高效液相色谱-串联质谱（ UPLC-MS／MS）同时检测猪肉中β-激动剂类、氯霉素类、阿维菌素类、磺胺类、氟喹诺酮类、硝基咪唑类、头孢类、四环素类、大环内酯类和聚醚类等10余类121种兽药的分析方法。样品经 Na2 EDTA-McIlvaine缓冲溶液（ pH＝4）和乙腈提取，无水硫酸钠盐析，上清液分为两组，分别用不同的 QuEChERS净化剂净化。使用电喷雾离子（ ESI）源，在多反应监测（ MRM）扫描模式下检测。5种兽药采用内标法定量，其余116种兽药采用外标法定量。121种兽药在0.02~40μg／L范围内线性关系良好（ r＞0.99），定量限（ S／N＝10）为0.05~10μg／kg。LOQ加标水平下，121种兽药中8种兽药的回收率为41.7％~59.6％，相对标准偏差为1.7％~13.5％；10种兽药的回收率为122.6％~163.2％，相对标准偏差为0.6％~14.8％；其余103种兽药的回收率为60.3％~118.3％，相对标准偏差为0.4％~16.7％。该方法可对性质差别大的多类别兽药同时进行分析，在节约成本和保证检测周期方面具有突出的优势。
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 dif-ferent mixed sorbents. The drugs were analyzed by UPLC-MS/MS in multiple reaction monito-ring( 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 corre-lation coefficients more than 0. 99. The limits of quantification( LOQs,S/N=10)were 0. 05-10μg/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.
参考文献
| [1] | Wiest, L.;Buleté, A.;Giroud, B.;Fratta, C.;Amic, S.;Lambert, O.;Pouliquen, H.;Arnaudguilhem, C..Multi-residue analysis of 80 environmental contaminants in honeys, honeybees and pollens by one extraction procedure followed by liquid and gas chromatography coupled with mass spectrometric detection[J].Journal of chromatography. A,201134(34):5743-5756. |
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