摘要
样品中的巴氯芬用0．01mol／LHCI溶液提取，提取液经WCX柱净化、富集后，进行液相色谱串联质谱（LC／MS-MS）分析。分析时采用BEHC_18色谱柱（100mm×2．1mm，1．7Bm），以0．10％甲酸水／甲醇作为流动相进行梯度洗脱，电喷雾正电子（ESI＋）模式电离，多反应监测（MRM）模式检测，内标法进行定量。结果表明：巴氯芬标准溶液在1．0～100．Oμg／L范围内，峰面积与含量呈线性相关。猪肉和猪尿中巴氯芬检出限分别为0．30μg／埏和0．10μg／L，两种样品中添加回收率在85％-110％之间，相对标准偏差（RsD）小于10％。
A simple and sensitive LC-MS/MS method for the determination ofbaclofen in pork and swine urine was developed. Samples were extracted with 0.01 mol/L HC1 solution, purified with a WCX cartridge and analyzed by LC/MS-MS on a Waters Acquity BEH C18 column with 0.10% formic acid in water/methanol as the mobile phase by means of gradient elution. Detection was carried out with an electrospray ionisation （ESI） probe and operated in the positive ion mode. Baclofen was quantified by the internal standard method. There was a good linearity in the range of concentrations between 1.0 and 100.0 μg/L. The limits of detection for baclofen were 0.30 μg/kg and 0.10 μg/L in pork and swine urine, respectively. The recoveries fi＇om spiked samples were in the range of 85% to 110% and the relative standard deviations were lower than 10%. These results showed that the method was simple, rapid, sensitive and reliable for monitoring residual baclofen in pork and swine urine.
出处
《肉类研究》
2013年第9期22-25,共4页
Meat Research
基金
宁波市科技局农业重大项目(2013C11003)
