| 引用本文: | 胡菲菲,胡延雷,苗庆柱,杨哲洲,张福利.HPLC检测磷酸可待因中的有关物质[J].中国现代应用药学,2019,36(17):2171-2176. |
| Hu Feifei,Hu Yanlei,Miao Qingzhu,Yang Zhezhou,Zhang Fuli.Determination of the Related Substance of Codeine Phosphate by HPLC[J].Chin J Mod Appl Pharm(中国现代应用药学),2019,36(17):2171-2176. |
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| 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。 |
| 关键词: 磷酸可待因 高效液相色谱法 有关物质 |
| DOI：10.13748/j.cnki.issn1007-7693.2019.17.011 |
| 分类号:R917.101 |
| 基金项目: |
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| Determination of the Related Substance of Codeine Phosphate by HPLC |
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Hu Feifei1, Hu Yanlei2, Miao Qingzhu2, Yang Zhezhou1, Zhang Fuli1
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1.Shanghai Institute of Pharmaceutical Industry, China State Institute of Pharmaceutical Industry, Shanghai 201203, China;2.China National Pharmaceutical Industry Corporation Ltd., Beijing 101301, China
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| 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. |
| Key words: codeine phosphate HPLC related substance |
