CAJ | 학술논문

实验建立了饲料中唑吡旦的液相色谱-串联质谱检测法。样品经1%三氯乙酸溶液提取，离心后经混合型阳离子交换MCX柱净化，氮气吹干，流动相溶解，液相色谱-串联质谱法进行测定，外标法定量。采用正离子扫描的方式进行仪器方法学研究，确定丰度比最高的2对离子作为监测离子，进行MRM模式定性定量分析。结果表明：该方法的检出限为0.02 mg/kg，定量限为0.05 mg/kg；唑吡旦浓度为2.0～500μg/L时线性关系良好，相关系数r=0.9998；添加浓度0.05～25 mg/kg，方法平均回收率为72.1%～85.4%，批内相对标准偏差为3.3%～7.5%。
실험건립료사료중서필단적액상색보-천련질보검측법。양품경1%삼록을산용액제취，리심후경혼합형양리자교환MCX주정화，담기취간，류동상용해，액상색보-천련질보법진행측정，외표법정량。채용정리자소묘적방식진행의기방법학연구，학정봉도비최고적2대리자작위감측리자，진행MRM모식정성정량분석。결과표명：해방법적검출한위0.02 mg/kg，정량한위0.05 mg/kg；서필단농도위2.0～500μg/L시선성관계량호，상관계수r=0.9998；첨가농도0.05～25 mg/kg，방법평균회수솔위72.1%～85.4%，비내상대표준편차위3.3%～7.5%。
A new liquid chromatography-tandem mass spectrometry (LC-MS/MS)method for determination of Zolpidem in animal feedstuff was reported.The samples were extracted with 1% trichloroacetic acid solution from analyte by ultrasonic.The extract was purified by passing through MCX solid-phase extraction cartridges.The elution was evaporated (50 ℃) and dulited to 2.0 mL,and then assayed by Liquid Chromatography-electrospray ionization tandem mass spectrometry.The limit of detection(LOD) was 0.02 mg/kg,and the limit of quantitation (LOQ) was 0.05 mg/kg.The calibration graph was linear between 2.0 μg/L and 500 μg/L for Zolpidem,and correlation coefficient was 0.9998. Recoveries of Zolpidem in different animal feedstuff were 72.1% ~85.4%,and inter-relative standard deviation(n=5)were 3.3%~7.5%,at spiked levels of 0.05~25 mg/kg.