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目的建立高效液相色谱-质谱联用(LC-MS)测定Beagle犬血清中樟柳碱的分析方法。方法采用沉淀及萃取相结合的方法提取样品,LC-MS分析方法,选择负离子测定模式,测定Beagle犬单剂量iv樟柳碱0.2mg/kg后樟柳碱的血药浓度。结果该方法线性、回收率和重现性良好,批内、批间变异系数均在10%以内,样品提取后24h内稳定,灵敏度可达到1ng/mL,出峰时间为3.1min,Cmax为(145.07±32.63)ng/mL,tmax为(0.04±0.06)h,AUC(0-t)为(361.10±26.01)mg·h/mL,CL为(5.56±0.41)L/h,t1/2为(1.67±0.34)h,Vd为(13.39±3.05)L。结论此方法简便、快速,专属性强,灵敏度高,能够准确测定血中氢溴酸樟柳碱,有实际意义。
Objective To establish a method for the determination of anisodine in serum of Beagle dogs by high performance liquid chromatography-mass spectrometry (LC-MS). Methods Samples were extracted by the method of precipitation and extraction. LC-MS analysis method was used to select anion measurement mode. The blood concentration of anisodine was measured after a single dose of iv anisodine 0.2 mg/kg in Beagle dogs. Results The linearity, recovery and reproducibility of the method were good. The intra-assay and inter-assay coefficients of variation were all within 10%. The samples were stable within 24 hours after extraction, the sensitivity was up to 1 ng/mL, the peak time was 3.1 min, and the Cmax was ( 145.07±32.63) ng/mL, tmax was (0.04±0.06) h, AUC(0-t) was (361.10±26.01) mg·h/mL, CL was (5.56±0.41) L/h, and t1/2 was (1.67±0.34)h, Vd is (13.39±3.05)L. Conclusion This method is simple, rapid, specific, high sensitivity, accurate determination of the anisodine hydrobromide in blood, has practical significance.