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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Reversed-phase high-performance liquid chromatographic separation of diastereomers of (R,S)-mexiletine prepared by microwave irradiation with four new chiral derivatizing reagents based on trichloro-s-triazine having amino acids as chiral auxiliaries and 10 others having amino acid amides
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Reversed-phase high-performance liquid chromatographic separation of diastereomers of (R,S)-mexiletine prepared by microwave irradiation with four new chiral derivatizing reagents based on trichloro-s-triazine having amino acids as chiral auxiliaries and 10 others having amino acid amides

机译：反相高效液相色谱分离（R，S）-美西汀的非对映异构体，方法是用四种基于三氯-s-三嗪的新型手性衍生试剂进行微波辐照，微波衍生有三种手性衍生试剂，其中三氯-s-三嗪具有氨基酸作为手性助剂，其余十种具有氨基酸酰胺

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摘要

A new series of chiral derivatizing reagents (CDRs) consisting of four dichloro-s-triazine reagents was synthesized by nucleophilic substitution of one chlorine atom in trichloro-s-triazine with amino acids, namely l-Leu, d-Phg, l-Val and l-Ala as chiral auxiliaries. Two other sets of CDRs consisting of four dichloro-s-triazine (DCT) and six monochloro-s-triazine (MCT) reagents were also prepared by nucleophilic substitution of chlorine atom(s) with different amino acid amides as chiral auxiliaries in trichloro-s-triazine and its 6-methoxy derivative, respectively. These 14 CDRs were used for the synthesis of diastereomers of (R,S)-mexiletine under microwave irradiation (i.e. 60s and 90s at 85% power (of 800W) using DCT and MCT reagents, respectively), which were resolved by reversed-phase high-performance liquid chromatography using C18 column and gradient eluting mixtures of methanol with aqueous trifluoroacetic acid (TFA) with UV detection at 230nm. The resolution (R_s), difference between retention times of resolved diastereomers (Δt) and retention factors (k) obtained for the three sets of diastereomers were compared among themselves and among the three groups. Explanations have been offered for longer retention times and better resolution of diastereomers prepared with DCT reagents in comparison of their MCT counterparts and, for the influence of hydrophobicity of the side chain R of the amino acid in the CDRs on retention times and resolution. The newly synthesized CDRs were observed to be superior as compared to their amide counterparts in terms of providing better resolution and cost effectiveness. The method was validated for limit of detection, linearity, accuracy and precision.
机译：通过亲和取代三氯-s-三嗪中的一个氯原子，由氨基酸（l-Leu，d-Phg，l-Val）合成了一系列由四种二氯-s-三嗪试剂组成的新的手性衍生试剂（CDR）和l-Ala作为手性助剂。还通过用不同的氨基酸酰胺亲和取代氯原子作为三氯环己烷中的手性助剂，制备了另外两种由四种二氯-s-三嗪（DCT）和六种一氯-s-三嗪（MCT）试剂组成的CDR。 s-三嗪及其6-甲氧基衍生物。这14个CDR用于在微波辐射下（即分别使用DCT和MCT试剂，在85％的功率（800W）下分别在60s和90s，功率为800W时）合成（R，S）-美西律汀的非对映异构体，并通过反相拆分高效液相色谱法，使用C18柱，梯度洗脱甲醇与三氟乙酸水溶液（TFA）的混合物，并在230nm处进行UV检测。比较了三组非对映异构体之间的分辨率（R_s），拆分的非对映异构体的保留时间之间的差异（Δt）和保留因子（k），并比较了三组非对映体。与它们的MCT对应物相比，已经提供了更长的保留时间和用DCT试剂制备的非对映异构体更好的分离度的解释，以及CDR中氨基酸侧链R疏水性对保留时间和分离度的影响。在提供更好的分辨率和成本效益方面，观察到新合成的CDR比其酰胺对应物更好。验证了该方法的检测极限，线性，准确性和精密度。

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