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[柠檬酸-锌(Ⅱ)介质中毛细管电泳法拆分D,L-异亮氨酸]

[Enantiomeric separation of D, L-isoleucine in citric acid-zinc (Ⅱ) medium by capillary electrophoresis].

作者信息

Chen Li, Zheng Ying, Chen Yufu, Yuan Qiuyue, Xie Tianyao

机构信息

School of Chemistry, Sun Yat-sen University, Guangzhou 510275, China.

出版信息

Se Pu. 2018 Jan 8;36(1):1-4. doi: 10.3724/SP.J.1123.2017.10008.

Abstract

The enantiomeric separation of unmodified D,L-isoleucine was achieved in citric acid-zinc(Ⅱ) medium by capillary electrophoresis (CE) with contactless conductivity detector (CD). In the conventional chiral separation methods of amino acid, a chiral complex used as the chiral selector was added into the eluent in order to yield a chiral environment. However, in this study a non-chiral solution, i. e. 2.8 mmol/L NaOH+0.8 mmol/L citric acid+2.0 mmol/L zinc acetate was used as the running buffer, and the citric acid-zinc(Ⅱ) acted the role of a chiral selector. Under the optimum experimental conditions:uncoated fused-silica capillary (45 cm×50 μm, =40 cm), separation voltage of +13 kV, electrokinetic injection of 11 kV×8 s, the enantiomers of D,L-isoleucine were baseline separated within 8 min with the resolutions () of 2.0. The calibration curve of each enantiomer showed good linearity in the range from 1.0 mg/L to 20 mg/L, with the limits of detection of 0.40 mg/L. The intra-and inter-day precisions were examined. The RSDs of peak area and migration time were found to be below 5.0% and 2.5% (=6), respectively, indicating good repeatability (intra-day) and reproducibility (inter-day) of the method. Interference experiment was also tested. As a result, other common amino acids did not interfere with the detection. The proposed method provided a potential new way to further investigate the enantioseparation of unmodified or native amino acids.

摘要

采用毛细管电泳(CE)结合非接触电导检测器(CD),在柠檬酸-锌(Ⅱ)介质中实现了未修饰的D,L-异亮氨酸的对映体分离。在传统的氨基酸手性分离方法中,为了产生手性环境,会向洗脱液中加入用作手性选择剂的手性配合物。然而,在本研究中,使用非手性溶液,即2.8 mmol/L NaOH + 0.8 mmol/L柠檬酸 + 2.0 mmol/L醋酸锌作为运行缓冲液,柠檬酸-锌(Ⅱ)起到了手性选择剂的作用。在最佳实验条件下:未涂层熔融石英毛细管(45 cm×50 μm,有效长度 = 40 cm),分离电压为 +13 kV,电动进样11 kV×8 s,D,L-异亮氨酸的对映体在8分钟内实现基线分离,分离度(Rs)为2.0。各对映体的校准曲线在1.0 mg/L至20 mg/L范围内呈良好线性,检测限为0.40 mg/L。考察了日内和日间精密度。发现峰面积和迁移时间的相对标准偏差分别低于5.0%和2.5%(n = 6),表明该方法具有良好的日内重复性和日间重现性。还进行了干扰实验。结果表明,其他常见氨基酸不干扰检测。该方法为进一步研究未修饰或天然氨基酸的对映体分离提供了一种潜在的新途径。

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