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目的采用柱前手性试剂衍生化反相高效液相色谱法测定L-去甲麻黄碱盐酸盐的光学纯度。方法采用手性衍生化试剂2,3,4,6-四乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯(GITC)对样品L-去甲麻黄碱盐酸盐进行柱前衍生化。衍生产物以乙腈-0.01mol.L-1磷酸二氢钾缓冲液(pH3.0)(40∶60)为流动相,在Agilent Zorbax C18(4.6mm×250mm,5μm)色谱柱上进行分离,流速为1.0mL.min-1,检测波长为210nm,柱温为30℃。结果D-去甲麻黄碱盐酸盐在0.3～5.0mg.L-1内线性关系良好,最低定量下限为0.3mg.L-1,平均回收率为98.0%,日内日间精密度考察中RSD均小于5.0%。结论该方法操作简便,衍生化产物稳定,结果准确,重现性好,灵敏度高,可用于L-去甲麻黄碱盐酸盐光学纯度的检查控制。
OBJECTIVE To determine the optical purity of L-norephedrine hydrochloride by precolumn derivatization with reversed-phase high performance liquid chromatography. Methods Pre-column derivatization of L-norephedrine hydrochloride was carried out using chiral derivatization reagent 2,3,4,6-tetraacetyl-β-D-glucopyranosyl isothiocyanate (GITC) The The derivative was separated on an Agilent Zorbax C18 (4.6 mm × 250 mm, 5 μm) column using acetonitrile-0.01 mol·L-1 potassium dihydrogen phosphate buffer (pH 3.0) (40:60) as the mobile phase. The flow rate 1.0mL.min-1, the detection wavelength was 210nm, the column temperature was 30 ℃. Results D-norephedrine hydrochloride showed a good linearity in the range of 0.3-5.0 mg · L-1 with the lowest limit of quantitation of 0.3 mg · L-1 and the average recovery of 98.0% Less than 5.0%. Conclusion The method is simple and convenient, the derivatized product is stable, the result is accurate, the reproducibility is good and the sensitivity is high. It can be used for the inspection and control of the optical purity of L-norephedrine hydrochloride.