超高效液相色谱-串联质谱法检测大鼠血浆中非洲防己碱  

Determination of columbamine in rat plasma by ultra-high performance liquid chromatography-tandem mass spectrometry

作　　者：谢海丽[1] 陈东鑫 董嫣文 王贤亲 XIE Hai-li;CHEN Dong-xin;DONG Yan-wen;WANG Xian-qin(Department of Pharmacy,Ningbo Medical Center(Group)Lihuili Hospital,Ningbo,Zhejiang 315040,China)

机构地区：[1]宁波市医疗中心李惠利医院药剂科,浙江宁波315040 [2]温州医科大学分析测试中心,浙江温州325035

出　　处：《中国卫生检验杂志》2020年第11期1300-1302,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立超高效液相色谱-串联质谱(UPLC-MS/MS)法检测大鼠血浆中非洲防己碱,并研究非洲防己碱的药代动力学及其绝对生物利用度。方法以格兰地新为内标,采用UPLC BEH C18柱(2. 1 mm×50 mm,1. 7μm)为分离柱,以乙腈-0. 1%甲酸为流动相,进行梯度洗脱,流速为0. 4 ml/min。大鼠血浆样本通过乙腈沉淀法去除蛋白,MRM模式监测定量,非洲防己碱m/z 338→322和内标m/z 322→307,正离子模式电喷雾离子源(ESI)。18只SD雄性大鼠用来药动学研究,分别静脉给药(0. 5 mg/kg和1. 0 mg/kg)和口服给药(10. 0 mg/kg)。结果在1 ng/ml^500 ng/ml内,该方法线性良好(r> 0. 995)。准确度在87. 5%~104. 3%,精密度<15%,基质效应在84. 2%~97. 7%,回收率≥78. 1%。结论该建立的UPLC-MS/MS方法简单、快速,并成功应用于非洲防己碱大鼠静脉和口服后的药代动力学,绝对生物利用率为15. 1%。Objective To establish a ultra-high performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS) method for the determination of columbamine in rat plasma,and study the pharmacokinetics and absolute bioavailability of columbamine. Methods Groenlandicine was used as internal standard,an UPLC BEH C18 column( 2. 1 mm × 50 mm,1. 7 μm) was used for chromatographic separation with the mobile phase consisted of acetonitrile and 0. 1% formic acid by gradient elution,the flow rate was set at 0. 4 ml/min. Proteins from rat plasma were removed by acetonitrile precipitation. Multiple reaction monitoring( MRM) mode was used for quantitative determination of columbamine in electrospray( ESI) positive interface,m/z 338→322 for columbamine and m/z 322→307 for internal standard. A total of 18 rats in the pharmacokinetic experiment were used for pharmacokinetics,intravenous administration( 0. 5 mg/kg and 1. 0 mg/kg),and oral administration( 10. 0 mg/kg). Results In the concentration of 1 ng/ml-500 ng/ml,the calibration curve was good linear( r > 0. 995),and the lower limit of quantification was 1. 0 ng/ml. The intra-day precision was less than 11%,the inter-day precision was less than 15%,the accuracy ranged from 87. 5% to 104. 3%,the recovery was ≥ 78. 1%,and the matrix effect was within84. 2%-97. 7%. Conclusion The UPLC-MS/MS method is simple and fast,and could be applied to the pharmacokinetic study of columbamine in rats after intravenous and oral administration;the absolute bioavailability is 15. 1%.

关 键 词：超高效液相色谱-串联质谱法 非洲防己碱 药代动力学 生物利用度 

分 类 号：O657.63[理学—分析化学]