摘要
目的:考察丙戊酸的衍生化条件,并建立测定丙戊酸血清浓度的方法。方法:血样采用α-溴苯乙酮衍生化,用高效液相色谱(HPLC)法进行测定。以丙戊酸衍生物产率为指标,采用单因素法考察反应温度、时间、三乙胺用量、衍生化试剂用量对丙戊酸衍生化的影响。结果:丙戊酸完全衍生化的条件为衍生化试剂用量400～600μg、三乙胺用量10～20μL、在45～60℃条件下反应20～60min。丙戊酸血药浓度在5.0～200.7μg·mL-1范围内线性关系良好(r=0.9999),方法回收率为99.80%～100.43%,日内与日间RSD≤4.45%。结论:衍生化试剂用量、三乙胺用量、反应温度和时间等对丙戊酸衍生化产率有较大的影响,在丙戊酸血清浓度测定中应加以控制。
OBJECTIVE： To investigate derivative conditions for determination of valproic acid, and to establish a method for the concentration determination of valproic acid in human serum. METHODS： The samples were derivatized with a-bromophenyl, and HPLC method was adopted. The effects of temperature and time of reaction, amount of triethylamine and derivatizing agent on derivatization of valproic acid were investigated by single-factor method with the yield of derivative as index. RESULTS： The condi- tions for full derivatization were as follows： derivatizing reagent was 400-600 μg, amount of triethylamine was 10-20μL, reac- tion temperature was 45-60 ℃ and reaction time was 20-60 min. The linear range of valproic acid was 5.0-200.7 μg·mL-1（r= 0.999 9）. The average recoveries were 99.80% -100.43%. RSD of intra-day and inter-day were no more than 4.45%. CONCLU- SION： Amount of derivatizing agent and triethylamine, temperature and time of reaction have significant impact on the yield of val- proic acid derivatization. The effects of them should be considered in determination of valproic acid in serum.
出处
《中国药房》
CAS
CSCD
2012年第42期3963-3965,共3页
China Pharmacy
基金
广西壮族自治区卫生厅自筹经费计划课题(Z2012523)
