色谱

色谱 ›› 2016, Vol. 34 ›› Issue (1): 103-107.DOI: 10.3724/SP.J.1123.2015.10013

• 研究论文 • 上一篇    下一篇

基于离子液体促进的手性配体交换毛细管电泳法分离分析去氧肾上腺素光学异构体

杨四梅, 张佳瑶, 李菲, 胡旭芳, 曹秋娥   

  1. 云南大学化学科学与工程学院, 教育部自然资源药物化学重点实验室, 云南 昆明 650091
  • 收稿日期:2015-10-12 出版日期:2016-01-08 发布日期:2012-08-01
  • 通讯作者: 曹秋娥
  • 基金资助:

    国家自然科学基金项目(21465025).

Separation and determination of optical isomers of phenylephrine by chiral ligand exchange capillary electrophoresis coupling with the promoting effect of ionic liquid

YANG Simei, ZHANG Jiayao, LI Fei, HU Xufang, CAO Qiue   

  1. Key Laboratory of Medicinal Chemistry for Nature Resource, Ministry of Education, School of Chemical Science and Technology, Yunnan University, Kunming 650091, China
  • Received:2015-10-12 Online:2016-01-08 Published:2012-08-01
  • Supported by:

    National Natural Science Foundation of China (No. 21465025).

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摘要：

基于非手性离子液体对手性配体交换的促进作用,建立了一种测定去氧肾上腺素手性异构体的毛细管电泳分离分析方法。在系统优化了电泳条件后,采用20 kV的分离电压、25 ℃的毛细管柱温、254 nm的检测波长以及5 s的压力(3447 Pa)进样时间,在添加4.0 mmol/L Cu(Ⅱ)、8.0 mmol/L L-脯氨酸(L-Pro)和15 mmol/L氯化-1-丁基-3-甲基咪唑([BMIM]Cl)的20 mmol/L Tris-H3PO4缓冲溶液(pH 5.4)中,R-去氧肾上腺素和S-去氧肾上腺素的分离度为1.42,峰面积与质量浓度分别在12.5~150.0 mg/L和15.0~150.0 mg/L范围内有线性关系。将该方法用于加标血液和尿液样品中R和S型去氧肾上腺素的测定,尿液中的加标回收率为93.7%~108.2%,相对标准偏差在3.18%(n=3)以内;血液中的加标回收率为91.4%~113.1%,相对标准偏差在4.82%(n=3)以内。

关键词: 光学异构体, 离子液体, 毛细管电泳, 去氧肾上腺素, 手性分离, 手性配体交换

Abstract:

A method for the separation and determination of optical isomers of phenylephrine was developed based on the promoting effect of non-chiral ionic liquid on chiral ligand-exchange capillary electrophoresis after the electrophoretic parameters were optimized systematically. R-phenylephrine and S-phenylephrine can be separated and determined effectively in 20 mmol/L Tris-H3PO4 buffer solution (pH 5.4) composed of 4.0 mmol/L Cu(Ⅱ), 8.0 mmol/L L-proline (L-Pro) and 15 mmol/L 1-butyl-3-methylimidazolium chloride ([BMIM]Cl) with the applied voltage of 20 kV, capillary temperature of 25 ℃, detection wavelength of 254 nm, and injection of 5 s at 3447 Pa. The resolution of R- and S-phenylephrines was 1.42. The linear ranges for the determination of R-phenylephrine and S-phenylephrine were 12.5-150 mg/L and 15.0-150 mg/L, respectively. The method has been satisfactorily used for the determination of R-phenylephrine and S-phenylephrine in the spiked blood and urine samples. The spiked recoveries in the urine sample were in the range of 93.7%-108.2% with the RSDs lower than 3.18%(n=3), and the spiked recoveries in the blood sample were in the range of 91.4% and 113.1% with the RSDs lower than 4.82%(n=3).

Key words: capillary electrophoresis, chiral ligand exchange, chiral separation, ionic liquid, optical isomers, phenylephrine

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