氢溴酸美沙芬含量及其杂质测定的研究

The assay of dextromethorphan hydrobromide and its impurities

目的：建立新的高效液相色谱测定氢溴酸美沙芬及其杂质含量的方法。方法：色谱条件以ＹＷＧＣ１８Ｈ３７为色谱柱；乙腈０．１ｍｏｌ·Ｌ－１磷酸二氢钾（５５∶４５）用磷酸调ｐＨ至４（含量）和２．５（杂质）为流动相；检测波长为２８０ｎｍ；并以对乙酰氨基酚为内标测定含量。结果：含量线性范围为８０～１２０μｇ·ｍｌ，回归方程Ｙ＝－０．０５９６＋０．１３１９Ｘ，ｒ＝０．９９９９（ｎ＝５），ＲＳＤ＝０．８２％。Ｎ，Ｎ二甲基苯胺测定最低浓度为０．１μｇ·ｍｌ－１。结论：含量测定方法简便、快速，结果准确。杂质测定灵敏度高，优于药典方法。

OBJECTIVE:To develop a HPLC new method for a assay of dextromethorphan hydrobromide and its impurities. METHODS: Chromatographed condition: column: YWG C 18 H 37 ; mobile phase: acetontitrile 0.1 mol·L -1 potassium dihydrogeu (KH 2 PO 4 ) solution (55∶45) adjusted pH with phosphoric acid to 4.0(assay) and 2.5 (impurity). Detected wavelengths: 280 nm; Internal standard: Paracetamol. RESULT: The linear range of the assay was 80～120 μg·ml -1 , and regression equation was Y=-0.059 6+0.131 9 X,r=0.999 9(n=5),RSD=0.82%。 The measurable lowest limit of N,N demethylaniline was 0.1 μg·ml -1 . CONCLUSION:The analytical method was simple, quick and precise. The measure ment of impurities was sensitive, and better than pharmacopeia methods.