RP-HPLC法同时测定人血浆中丙戊酸钠及其代谢产物的浓度
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篇名: RP-HPLC法同时测定人血浆中丙戊酸钠及其代谢产物的浓度
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摘要: 目的:建立同时测定人血浆中丙戊酸钠(VPA)及其代谢产物2-丙基-2-戊烯酸(2-ene-VPA)浓度的方法。方法:血浆样品经环己烷沉淀蛋白后,用2,4′ -二溴苯乙酮进行衍生化,以正辛酸为内标,采用反相高效液相色谱法测定。色谱柱为Zorbax SB-C18,流动相为乙腈-水(65 ∶ 35,V/V),流速为1 mL/min,柱温为35 ℃,紫外检测波长为258 nm,进样量为20 μL。结果:VPA、2-ene-VPA血药浓度分别在5.0~200.0、0.5~20.0 μg/mL范围内线性关系良好(r均为0.999 9,n=5),定量下限分别为5.0、0.5 μg/mL;日内、日间RSD均小于5%,方法回收率分别为95.99%~98.80%、97.40%~98.17%,提取回收率分别为80.46%~86.23%、80.45%~85.61%。采用该法测得10例癫痫患儿VPA血药浓度为27.4~93.2 μg/mL,2-ene-VPA血药浓度为0.85~3.94 μg/mL。结论:该方法操作简便、专属性强,可用于VPA血药浓度检测及药动学研究。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of sodium valproate (VPA) and its metabolite 2-propyl-2-pentenoic acid (2-ene-VPA) in human plasma.  METHODS: Plasma sample was extracted with cyclohexane and experienced derivatization with 2,4′ -dibromoacetophenone using n-octanoic acid as an internal standard. RP-HPLC method was adopted. The determination was performed on Zorbax SB-C18 column with mobile phase consisted of acetonitrile-water (65 ∶ 35,V/V) at the flow rate of 1 mL/min. The column temperature was set at 35 ℃, and UV  dectection wavelenth was set at 258 nm. The sample size was 20 μL. RESULTS: The linear range of VPA and 2-ene-VPA were 5.0-200.0, 0.5-20.0 μg/mL (r=0.999 9,n=5). The limits of quantification were 5.0, 0.5 μg/mL. RSDs of inter-day and intra-day were all lower than 5%. Method recoveries were 95.99%-98.80% and 97.40%-98.17%, and extraction recoveries were 80.46%-86.23% and 80.45%-85.61%. The plasma concentrations of VPA in 10 epileptic children were 27.4-93.2 μg/mL, and those of 2-ene-VPA were 0.85-3.94 μg/mL, respectively. CONCLUSIONS: The method is simple, specific and suitable for plasma concentration determination and pharmacokinetic study of VPA.
期刊: 2017年第28卷第5期
作者: 张玲敏,谢娟,李龙宽,廖荣华,邱钟燕
AUTHORS: ZHANG Lingmin,XIE Juan,LI Longkuan,LIAO Ronghua,QIU Zhongyan
关键字: 丙戊酸钠;2-丙基-2-戊烯酸;反相高效液相色谱法;衍生化;血药浓度
KEYWORDS: Sodium valproate; 2-propyl-2-pentenoic acid; RP-HPLC; Derivatization; Plasma concentration
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