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Fluorimetric determination of the enantiomers of vigabatrin, an antiepileptic drug, by reversed‐phase HPLC with a novel diastereomer derivatization reagent
Biomedical Chromatography ( IF 1.8 ) Pub Date : 2020-12-29 , DOI: 10.1002/bmc.5060
Shusuke Uekusa 1, 2 , Mayu Onozato 1 , Tatsuya Sakamoto 1 , Maho Umino 1 , Hideaki Ichiba 1 , Takeshi Fukushima 1
Affiliation  

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 ~0.80 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.

中文翻译:

新型非对映异构体衍生化试剂反相HPLC荧光法测定抗癫痫药Vigabatrin对映体

在此,使用新设计和合成的荧光衍生化试剂2,5-二氧杂吡咯烷-1-基(4- { [(2-硝基苯基)磺酰基]氧基} -6-(3-氧代吗啉代)喹啉-2-羰基)脯氨酸盐[Ns-MOK-(R)-或(S)-Pro-OSu]。在60°C下用Ns‐MOK‐(R)‐Pro‐OSu衍生化VB的过程中,被引入以保护酚羟基的Nosyl(Ns)基团在30分钟内释放出来以生产MOK‐(R)-Pro-VB,在448 nm处以荧光法检测到,激发波长为333 nm。由于Ns‐MOK‐(R)‐Pro‐OSu具有光学活性D‐脯氨酸结构,因此VB对映异构体在十八烷基硅胶(ODS)色谱柱上分离,分离度为5.57 。使用逐步梯度洗脱,在40分钟内在ODS色谱柱上实现了MOK-(R)-Pro-(R)-和-(S)-VB对映异构体的完全分离,并且在PDS上的检测限分别为〜0.80和0.37 pmol列。用阴离子交换盒固相萃取后,所建议的采用荧光检测方法的HPLC已成功用于测定VB加标的人血清中的VB对映异构体。
更新日期:2020-12-29
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