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首页> 外文期刊>Canadian Journal of Chemistry >Analysis of ketoprofen enantiomers in human and rat plasma by hollow-fiber-based liquid-phase microextraction and chiral mobile-phase additive HPLC
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Analysis of ketoprofen enantiomers in human and rat plasma by hollow-fiber-based liquid-phase microextraction and chiral mobile-phase additive HPLC

机译：中空纤维液相微萃取和手性流动相添加剂HPLC分析人和大鼠血浆中的酮洛芬对映体

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摘要

A simple, inexpensive, and efficient preconcentration and cleanup three-phase hollow fiber liquid-phase microextraction method (HF-LPME) was developed for the extraction of the anti-inflammatory ketoprofen (KTP) from human and rat plasma and HPLC enantioseparation of its enantiomers using vancomycin as a chiral mobile-phase additive with an achiral C8 column. The effects of different parameters influencing the efficiency of extraction were optimized for aqueous samples. Under optimized conditions, KTP enantiomers were extracted from 0.5 mL of plasma diluted to 5 ml with salinated and acidified deionized water (pH = 2) with 25 μL of alkalinized acceptor phase (pH = 11) during 30 min at room temperature. The mean recoveries of (-)-(R)- and (+)-(S)-KTP were 72.8% and 70.9%, respectively. The quantification limit was 20 ng/mL with linear response over the 20-2000 ng/mL concentration range for both enantiomers. Assay precision was studied within-day and between-day using 100 ng/mL KTP solutions. For both KTP enantiomers, relative standard deviations were lower than 12%. The proposed microextraction method was applied for the extraction of KTP enantiomers from human and rat plasma samples after oral administration of pure (±)-KTP in 4 mg/kg dosage for rats and 50 mg dosage for humans to assess the enantiospecific bioavailability of KTP enantiomers in their plasma. In vivo inversion studies revealed that the bioavailability of S-KTP is higher than that of the R enantiomers in rat, but they are similar in human plasma. The developed method showed that HF-LPME is a promising technique for sample preparation for the analyses of chiral drugs in biological samples.
机译：开发了一种简单，廉价，有效的预浓缩和净化三相中空纤维液相微萃取方法（HF-LPME），用于从人和大鼠血浆中提取抗炎性酮洛芬（KTP），并对其对映体进行HPLC对映分离使用万古霉素作为非手性C8色谱柱的手性流动相添加剂。针对水性样品优化了不同参数对萃取效率的影响。在最佳条件下，在室温下30分钟内，用含25μL碱化受体相（pH = 11）的盐化和酸化去离子水（pH = 2）从0.5 mL血浆稀释至5 ml血浆中提取KTP对映体。 （-）-（R）-和（+）-（S）-KTP的平均回收率分别为72.8％和70.9％。两种对映体的定量限为20 ng / mL，线性响应在20-2000 ng / mL的浓度范围内。使用100 ng / mL KTP溶液在一天之内和一天之间进行测定精度的研究。对于两种KTP对映体，相对标准偏差均低于12％。拟议的微萃取方法应用于口服和口服大鼠纯净（±）-KTP，大鼠剂量为4 mg / kg，人类剂量为50 mg，从人和大鼠血浆样品中提取KTP对映体，以评估KTP对映体的对映体生物利用度在他们的血浆中。体内转化研究表明，S-KTP在大鼠体内的生物利用度高于R对映异构体，但在人血浆中却相似。所开发的方法表明，HF-LPME是用于分析生物样品中手性药物的样品前处理的有前途的技术。

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