摘要
目的建立测定精神分裂症合并2型糖尿病患者血浆中沙格列汀浓度的方法。方法血浆样品0．2mL用醋酸乙酯一二氯甲烷（体积比4：1）萃取，西他列汀作为内标，采用LC．MS／MS法测定。色谱柱为Agilent Eclipse plus C18（4．6mm×150Mm，3．5μm），以甲醇-水（体积比95：5，含0．005mol／L甲酸铵和质量分数0．1％甲酸）为流动相，流速为0．5mL／min，柱温为40℃；质谱条件采用ESI离子源，检测方式为正离子电离，多重反应监测（MRM），用于定量分析的离子反应分别为m／z316．2→180．2（沙格列汀）与m／z 408．1→235．1（西他列汀）。结果沙格列汀在0．5—100μg／L（r2=0．998）范围内线性良好，其平均回收率在79．24％以上，日内、日间精密度分别小于8．30％与12．92％（次低浓度点）。结论本试验建立的沙格列汀血药浓度的测定方法简便、快速、准确、灵敏，可用于临床研究中沙格列汀的药动学研究。
Objective To establish a LC-MS/MS method for the determination of saxagliptin in plasma samples of Chinese male schizophrenia patients complicated with type 2 diabetes （T2DM）. Methods Saxagliptin was extracted from plasma by ethyl acetate-dichloromethane （ 4 ： 1 ）. Then saxagliptin was determined by LC-MS/MS using sitagliptin as internal standards respectively. Separation carried on a Agilent Eclipse plus C1s（ 150 mm×4.6 mm, 5 μm） column with a mobile phase of methanol-0.005 mol/L ammonium formate aqueous solution with 0.1% formic acid （95：5 ） at the flow rate of 0.5 mL/min. The column temperature was set at 40℃. ESI source was applied and operated in positive ion mode. Quantitative determination was performed using multiple reaction monitoring （MRM） of m/z 316.2→180.2 for saxagliptin and m/z 408.1→235.1 for sitagliptin. Results Saxagliptin exhibited good linearity in the range of 0.5-100 μg/L （r2= 0.998）. The extraction recovery for saxagliptin was more than 79.24%, while the intra-day and inter-day precision （RSD） were lower than 8.30% and 12.92%, respectively. Conclusion The method is simple, rapid, accurate, and sensitive for determination of saxagliptin in human plasma, which can be applied to the clinical pharmacokinetic-pharmacodynamic study of saxagliptin among schizophrenia patients complicated with T2DM.
出处
《今日药学》
CAS
2014年第8期556-559,563,共5页
Pharmacy Today
基金
广东省药学会医院药学研究基金(编号:2012C01)
