摘要
目的：建立高效液相-质谱/质谱分析方法测定人血清中的氟桂利嗪，并用于研究健康受试者静脉滴注盐酸氟桂利嗪注射液后的药动学。方法：血清经1mol·L^-1氢氧化钠溶液碱化后，正己烷-异丙醇（95：5）提取，采用Shimadzu ODS柱（150mm×4.6mm，5μm）为分析柱，甲醇-醋酸铵溶液（10mmol·L^-1，冰醋酸调pH3.5）（75：25）为流动相，流速1.0mL·min^-1，柱后分流，0.2mL·min^-1进入质谱，柱温35℃。质谱检测方式为多反应离子监测，选择监测的离子为m/z 203.4→m/z 183.1（氟桂利嗪）和m/z 285.4→m/z 193.2（地西泮）。结果：氟桂利嗪的线性范围为0.5～500μg·L^-1（r=0.9998），血清中氟桂利嗪的检测限达0.1μg·L^-1（S/N〉3），回收率大于85％。结论：本法简便，准确，灵敏度高，适用于氟桂利嗪的药动学研究。
OBJECTIVE An HPLC-MS/MS method was established for the study of pharmacokinetics of flunarizine in human. METHODS Diazepam was used as internal standard. After adding diazepam, the serum was alkalized with 1 mol·L^-1 sodium hydroxide solution and extracted with n-hexane-isopropanol （95：5）. The separation was carried out on a Shimadzu ODS column （150 mm× 4. 6 mm, 5/μm） at 35 ℃. The mobile phase was methanol-10 mmol·L^-1 ammonium acetate （pH 3.5 adjusted by acetic acid） （75：25）, running at a flow rate of 1.0 mL·min^-1. After separation, the mobile phase was splitted and 0. 2 mL,min-1 was into MS. HPLC-MS/MS was performed in the MRM mode using target ions at 7n/z 203.4→m/z 183.1 for flunarizine and rn/z 285.4→m/z 193. 2 for diazepam. RRESULTS The linear calibration curve was obtained in the concentration range of 0. 5～500 μg·L^-1 （r = 0. 999 8）. The detection limit of flunarlzine in serum was 0.1μg·L^-1. The average recovery was more than 85%. CONCLUSION The assay was proved to be sensitive, accurate and convenient. The method can be used for the pharmacokinetic research of flunarizine.
出处
《中国医院药学杂志》
CAS
CSCD
北大核心
2007年第12期1676-1678,共3页
Chinese Journal of Hospital Pharmacy
