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首页> 外文期刊>Biomedical Chromatography: An International Journal Devoted to Research in Chromatographic Methodologies and Their Applications in the Biosciences >Fluorimetric determination of the enantiomers of vigabatrin, an antiepileptic drug, by reversed-phase HPLC with a novel diastereomer derivatization reagent
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Fluorimetric determination of the enantiomers of vigabatrin, an antiepileptic drug, by reversed-phase HPLC with a novel diastereomer derivatization reagent

机译：用新型非对映异构体衍生化试剂的反相HPLC荧光测定抗癫痫药物，抗癫痫药物，抗癫痫药物的映体

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摘要

Herein, determination of an antiepileptic drug, (±)-vigabatrin (VB), was performed by reversed-phase HPLC with fluorimetric detection using a newly designed and synthesized fluorescence derivatization reagent, 2,5-dioxopyrrolidin-1-yl (4-{[(2-nitrophenyl)sulfonyl]oxy}-6-(3-oxomorpholino)quinoline-2-carbonyl)prolinate [Ns-MOK-(R)- or (S)-Pro-OSu]. During the derivatization of VB with Ns-MOK-(R)-Pro-OSu at 60°C, the nosyl (Ns) group, which was introduced to protect a phenolic hydroxy group, was released within 30 min to produce MOK-(R)-Pro-VB, which was detected fluorimetrically at 448 nm with an excitation wavelength of 333 nm. The VB enantiomers were separated on an octadecylsilica (ODS) column with a resolution value of 5.57, because Ns-MOK-(R)-Pro-OSu bears an optically active D-proline structure. A complete separation of MOK-(R)-Pro-(R)- and -(S)-VB enantiomers was achieved on the ODS column within 40 min using stepwise gradient elution, and the detection limits were approx0.80 and 0.37 pmol on the column, respectively. The proposed HPLC with fluorimetric detection method was successfully used for determining VB enantiomers in VB-spiked human serum following solid-phase extraction with an anion-exchange cartridge.
机译：在此，通过使用新设计的和合成的荧光衍生试剂，2,5-二氧吡咯烷蛋白-1-基（4-（ [（2-硝基苯基）磺酰基]氧气}} -6-（3-氧代）喹啉-2-羰基）脯氨酸[ns-mok-（r） - 或（s）-pro-osu]。在60℃的NS-MOK-（R）-PRO-OSU的VB的衍生化期间，引入保护酚醛羟基的亚硒（NS）基团在30分钟内释放以产生MOK-（R. ）-Pro-Vb，其在448nm处以激发波长为333nm的荧光检测。 VB对映异构体在十八烷基硅（ODS）塔上分离，分辨率值为5.57，因为NS-MOK-（R）-Pro-OSU承受光学活性的D-脯氨酸结构。使用逐步梯度洗脱在40分钟内在ODS柱内完成Mok-（R） - 和 - （S）-VB对映体的完全分离，并且检测限量约为0.80和0.37pmol分别列。提出的具有荧光检测方法的HPLC成功用于在用阴离子交换盒之后在固相萃取后确定VB掺入人血清中的VB对映体。

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