Cao Yafei, Kang Jian, Chang Qiaoying, Hu Xueyan, Wang Zhibin, Fan Chunlin, Wang Minglin
Se Pu. 2015 Feb;33(2):132-9. doi: 10.3724/sp.j.1123.2014.10022.
A rapid and sensitive method has been developed for the simultaneous determination of 50 veterinary drugs (including macrolides, quinolones, sulfonamides, and tetracyclines) in cheese using a modified QuEChERS method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). After adding Na2EDTA buffer solution and ceramic homogenizer, the cheese sample was extracted by 5% (v/v) acetic acid-acetonitrile, sodium chloride and anhydrous sodium sulfate were used for salting-out process. The resulting supernatant solution was purified by C18 sorbent and the re-dissolved solution was analyzed by LC-MS/MS under dynamic multi-reaction monitoring (dynamic MRM) mode via positive electrospray ionization with a ZORBAX-SB-C18 column. The limits of quantification (LOQ, S/N= 10) of the target compounds ranged from 0. 05 µg/kg to 20 µg/kg in cheese. At spiked levels of 20, 50, 100 µg/kg (n =6) , the percentages of drug with a recovery between 70% and 120% were 94%, 92%, and 96%, respectively. The relative standard deviations (RSDs) were between 1% and 14%. This method has been applied to determine seven real samples from markets. Roxithromycin and flumequine have been detected in two samples separately. The results demonstrated that this simple, rapid and accurate method is suitable for the detection of multi-class veterinary drugs in cheese.
已开发出一种快速灵敏的方法,用于同时测定奶酪中50种兽药(包括大环内酯类、喹诺酮类、磺胺类和四环素类),该方法采用改良的QuEChERS方法结合液相色谱-串联质谱法(LC-MS/MS)。加入Na2EDTA缓冲溶液并用陶瓷均质器处理后,用5%(v/v)乙酸-乙腈提取奶酪样品,使用氯化钠和无水硫酸钠进行盐析过程。所得上清液用C18吸附剂净化,重新溶解后的溶液通过ZORBAX-SB-C18柱在动态多反应监测(动态MRM)模式下,经正电喷雾电离,采用LC-MS/MS进行分析。目标化合物在奶酪中的定量限(LOQ,S/N = 10)为0.05 μg/kg至20 μg/kg。在加标水平为20、50、100 μg/kg(n = 6)时,回收率在70%至120%之间的药物百分比分别为94%、92%和96%。相对标准偏差(RSD)在1%至14%之间。该方法已应用于测定来自市场的7个实际样品。在两个样品中分别检测到罗红霉素和氟甲喹。结果表明,这种简单、快速且准确的方法适用于检测奶酪中的多类兽药。