摘要
目的 建立测定人血浆中多奈哌齐的HPLC MS(TOF)法。方法 血浆中加入内标氯雷他定后经碱化以异丙醇 正己烷 (3∶97)提取血浆样品 ,用LC MS(TOF)联用技术 ,以电喷雾 (ESI)作为接口技术 ,选择多奈哌齐的准分子离子 ([M +H]+ ,m z 380 )和内标氯雷他定的准分子离子 ([M +H]+ ,m z 383)作为测定离子 ,测定人血浆中多奈哌齐的浓度。结果 多奈哌齐的回归方程 :As Ai=0 0 137+0 10 5 6C ,r =0 9998;线性范围为 0 1～ 15 μg·L- 1 ,定量限为 0 1μg·L- 1 ,方法回收率和提取回收率均大于 90 %。结论 该测定方法灵敏度高、专属性好、快速 。
Aim To establish a sensitive and specific liquid chromatography mass spectrometry (time of flight) [LC MS (TOF)] method for the determination of donepezil in human plasma after an oral administration of 5 mg donepezil hydrochloride tablet. Methods Alkalized plasma was extracted with isopropanol n hexane (3∶97) and loratadine was used as internal standard. Solutes were separated on a C 18 column with a mobile phase of methanol acetate buffer (pH 4 0) (80∶20). Detection was performed on a time of flight mass spectrometry equipped with an ESI interface and operated in positive ionization mode. Donepezil quantitation was realized by computing the peak area ratio (donepezil loratadine) (donepezil m/z 380[M+H] + and loratadine m/z 383[M+H] +) and comparing them with calibration curve ( r =0 9998). Results The linear calibration curve was obtained in the concentration range of 0 1-15 μg·L -1 . The detection limit of donepezil was 0 1 μg·L -1 . The average recovery was more than 90%. The intra and inter run precision was measured to be below 15% of RSD. Conclusion The method is sensitive, simple and rapid, so, it can meet the need of the studies on the pharmacokinetics and bioavailability of donepezil.
出处
《药学学报》
CAS
CSCD
北大核心
2003年第3期203-206,共4页
Acta Pharmaceutica Sinica
