HPLC检测磷酸可待因中的有关物质

Determination of the Related Substance of Codeine Phosphate by HPLC

关键词:  磷酸可待因  高效液相色谱法  有关物质

Key words:  codeine phosphate  HPLC  related substance

摘要:

目的 建立HPLC检测磷酸可待因中的有关物质。方法 采用以十八烷基硅烷键合硅胶为填充剂的色谱柱，以缓冲溶液（0.2%磷酸二氢钾1%庚烷磺酸钠的水溶液，磷酸调pH至3.2±0.2）-甲醇（7：3）为流动相A；以流动相A-乙腈（6：4）作为流动相B，采用梯度洗脱；流速1.0 ml·min^-1，检测波长245 nm，柱温40℃。结果 该方法主成分与各杂质（A~K）间分离度>1.5。主成分及其各杂质在各自浓度范围内呈现良好的线性关系（r>0.999）；平均回收率为96.7%~103.8%，RSD为1.4%~6.0%。结论 该方法操作简单、专属性好、重复性好、准确度高，适用于磷酸可待因的有关物质的测定。

Abstract:

OBJECTIVE To establish an HPLC method for determination of the related substances in codeine phosphate. METHODS The test was based on an octadecylsilyl silica gel column; the mobile phase A consisted of 0.2% potassium dihydrogen phosphate and 1% sodium heptanesulfonate (pH was adjusted to 3.2±0.2 with phosphoric acid)-methanol(7:3), the mobile phase B consisted of mobile phase A and acetonitrile(6:4), with gradient elution at the flow rate of 1.0 mL·min^-1; the detection wavelength was 245 nm; the column temperature was 40℃. RESULTS The separation between the main component of the method and each impurity(A-K) were >1.5. The calibration curves of codeine and known impurities were linear in the self-concentration range; and the average recovery rates(n=9) were in the range of 96.7%-103.8% while RSDs were in th range of 1.4%-6.0%. CONCLUSION The method is improved with good specificity and linearity. The self-control method for proposed main component with correction factors is suitable for the quality control of this drug.