超高效液相色谱串联质谱检测动物组织中卡马西平及其代谢物的残留量

Simultaneous Determination of Carbamazepine and Its Metabolites in Animal Matrix Using Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

卡马西平为治疗癫痫和三叉神经痛等精神疾病药物,但其具有刺激抗利尿激素释放,可引起水钠潴留副作用。水钠潴留可造成组织水肿,体重异常,为养殖环节非法注水提供了保水抗利尿的可能,因此检测动物组织中卡马西平对打击非法注水意义重大。本文采用超高效液相色谱串联质谱建立动物组织中卡马西平及其代谢物环氧卡马西平残留检测方法。样品经过0.2%甲酸乙腈提取、Oasis PRi ME HLB柱净化后,经Acquity UPLC BEH C18(100 mm×2.1 mm,1.7μm)分离,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,正离子MRM信号采集模式,两种药物能在8 min内分离完好,在1.0~50.0μg/L浓度范围内,线性良好,相关系数均在0.999以上;方法定量限均为1.0μg/kg,通过1.0、10、20μg/kg三个浓度的加标回收实验表明,回收率为72.3%~106.8%,RSD%值为1.43%~10.3%。该方法为防范动物产品中非法药物添加和注水等违法行为提供了一定的技术参考。

Carbamazepine is a drug for the treatment of psychiatric illnesses, such as epilepsy, trigeminal neuralgia and so on. However, it also can stimulate the release of antidiuretic hormone, causing side effect of water-sodium retention. Water-sodium retention can lead to tissue edema and weight disorders, which provides the possibility of water retention and antidiuretic by illegal water injection in the breeding process. Therefore, it is of great significance to detect carbamazepine in animal tissues for cracking down on illegal water injection. A multiresidue method based on ultra performance liquid chromatography tandem mass spectrometry was developed for the determination of carbamazepine and its metabolites in animal matrix. In this method, samples were extracted by acidified acetonitrile, and purified by Oasis PRi ME HLB SPE column, and then carbamazepine and its metabolites were analyzed by Acquity UPLC BEH C18 column（100 mm×2.1 mm, 1.7 μm） using methanol and 0.1% formic acid as the mobile phases. The signals were acquired through the MRM mode. All analytes could be well-separated by a gradient program during 8 minutes. The calibration curves of carbamazepine and its metabolites had a good linear in a concentration range of 1.0-50.0 μg/L with the correlation coefficient more than 0.999, and the limits of quantitation were all less than 1.0 μg/kg in animal matrix. The recoveries of 1.0, 10, 20 μg/kg fortified samples ranged from 72.3% to 106.8%, with RSDs of 1.43% to 10.3%. The new method provides a certain reference for the prevention of illicit drug addition and water injection in animal products.