基于非手性离子液体对手性配体交换的促进作用,建立了-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20kV的分离电压、25℃的毛细管柱温、254nm的检测波长以及5s的压力(3447Pa)进样时间,在添加4.0mmol/LCu(Ⅱ)、8.0mmol/LL-脯氨酸(L—Pro)和15mmol/L氯化-1-丁基-3-甲基咪唑([BMIM]C1)的20mmol/L Tris—H3PO4缓冲溶液(pH5.4)中,R-去氧肾上腺素和g去氧肾上腺素的分离度为1.42,峰面积与质量浓度分别在12.5~150.0mg/L和15.0~150.0mg/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。
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 system- atically. 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 !-butyl-3-methylimidazolium chloride ( [ BMIM 1 C1) with the applied voltage of 20 kV, capillary temperature of 25 0(;, detection wavelength of 254 nm, and injection of 5 s at 3 447 Pa. The resolution of R- and S-phenylephrines was 1.42. The linear ran- ges 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 recov- eries 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 9 1. 4% and [ 13. 1% with the RSDs lower than 4.82% ( n = 3).