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 -0.01 mol· L -1 磷酸二氢钾缓冲液（ pH 3.0 ）（ 40 ∶ 60 ）为流动相，在 Agilent Zorbax C18(4.6 mm × 250 mm ， 5 μm) 色谱柱上进行分离，流速为 1.0 mL·min-1 ，检测波长为 210 nm ，柱温为 30 ℃。 结果 <>D- 去甲麻黄碱盐酸盐在 0.3 ～ 5.0 mg· L -1 内线性关系良好，最低定量下限为 0.3 mg· 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。
Abstract
OBJECTIVE To establish a chiral precolumn derivatization method for optical purity test of L-norephedrine hydrochloride. METHODS The enantiomers of norephedrine hydrochloride were derivatized with a pre-column chiral derivatization reagent 2，3，4，6-tetra-O-acetyl-β-D-glucopyranosyl -isothiocyanate (GITC). The diastereoisomers produced were separated on an Agilent Zorbax C18 column (4.6 mm×250 mm，5 μm) with a mobile phase consisting of acetonitrile -0.01 mol·L-1 phosphate buffer (pH 3.0) (40∶60). The flow rate was set at 1.0 mL·min-1 and the detection wavelength was set at 210 nm. RESULTS The method was linear in the range of 0.3-5.0 mg·L-1 for the D-norephedrine hydrochloride. The lower limit of detection for D-norephedrine hydrochloride was 0.1 mg·L-1 and the lower limit of quantification was 0.3 mg·L-1. The inter- and intra-day precision (RSD) was below 5.0% and the average recovery was 98.0%. CONCLUSION The method is simple, accurate and suitable for the quality control of optical purity of L-norephedrine hydrochloride.
关键词
去甲麻黄碱 /
光学杂质 /
高效液相色谱法 /
柱前衍生化
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Key words
norephedrine /
optical impurity /
HPLC /
pre-column derivatization
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参考文献
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（收稿日期： 2008-12-10 ）
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