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目的:建立生物样品中敌鼠和氯鼠酮的高效液相色谱/质谱联用同时测定方法。方法:全血样品经甲醇+乙腈(50+50,v/v)提取,尿液样品经Oasi sHLB固相萃取小柱净化富集后,采用Extend C18柱(150 mm×4.6 mm i.d.,5μm),以乙酸铵-乙酸(0.02 mol/L,pH 5.5)+甲醇(15+85,v/v)为流动相,采用选择离子监测(SIM)技术在电喷雾电离(ESI)负离子模式下同时检测,敌鼠和氯鼠酮的定量检测离子分别为m/z 339.0[M-H]-和m/z 373.0[M-H]-,外标法定量。结果:针对全血样品,敌鼠在2.0~500.0μg/L,氯鼠酮在1.0~200.0μg/L范围内呈良好线性关系,敌鼠和氯鼠酮的回收率分别在92.1%~94.5%和93.0%~94.2%范围,RSD分别小于7.5%和6.5%,检出限分别为2.0μg/L和1.0μg/L。针对尿液样品,敌鼠在0.5~100.0μg/L,氯鼠酮在0.2~40.0μg/L范围内呈良好线性关系,敌鼠和氯鼠酮的回收率分别为95.2%~97.0%和92.0%~96.5%,RSD分别小于6.0%和7.5%,检出限分别为0.5μg/L和0.2μg/L。结论:本方法简便、灵敏、重现性好,能满足敌鼠和氯鼠酮中毒病人的临床诊断检测要求。
OBJECTIVE: To establish a simultaneous HPLC / MS method for the simultaneous determination of dipyridamole and chloroketone in biological samples. Methods: Whole blood samples were extracted with methanol and acetonitrile (50 + 50, v / v). The urine samples were purified by Oasi sHLB solid phase extraction cartridges. The samples were extracted on an Extend C18 column (150 mm × 4.6 mm id, The mobile phase was eluted with ammonium acetate-acetic acid (0.02 mol / L, pH 5.5) + methanol (15 + 85, v / v) using ion selective ion monitoring (SIM) , And the quantitative detection ions for the antagonist and the chloride were m / z 339.0 [MH] - and m / z 373.0 [MH] -, respectively, and were quantified by external standard method. Results: For the whole blood samples, the linear range was 1.0-500.0 μg / L for rival rats and 1.0-200.0 μg / L for chlorothalonil, and the recovery rates for both anti-rat and rat were between 92.1% and 94.5% And 93.0% ~ 94.2% respectively. The RSDs were less than 7.5% and 6.5%, respectively. The detection limits were 2.0μg / L and 1.0μg / L, respectively. For the urine samples, the linear range of 0.5 ~ 100.0μg / L was in the range of 0.5 ~ 100.0μg / L against the rat and the range of 0.2 ~ 40.0μg / L was in the range of 0.2 ~ 40.0μg / L. The recoveries were between 95.2% ~ 97.0% and 92.0% % ~ 96.5%, RSD less than 6.0% and 7.5%, respectively. The limits of detection were 0.5μg / L and 0.2μg / L, respectively. Conclusion: The method is simple, sensitive and reproducible. It can meet the clinical diagnostic test requirements of the patients with poisoned rats and the rats with.