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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 |
| TITLE： | |
| 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 |
| 阅读数： | 288 次 |
| 本月下载数： | 13 次 |
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