中国药物警戒 ›› 2015, Vol. 12 ›› Issue (7): 398-401.

• 质量与工艺研究 • 上一篇    下一篇

硝酸咪康唑栓剂近红外快速定量方法的建立

王小亮, 张秉华, 冯润东, 衷红梅, 席志芳   

  1. 陕西省食品药品检验所,陕西 西安 710065
  • 收稿日期:2015-09-01 修回日期:2015-09-01 出版日期:2015-07-08 发布日期:2015-09-02
  • 作者简介:王小亮,女,硕士,主管药师,药物分析。

Construction of a Fast Quantitative Method for Miconazole Nitrate Suppository Using Near Infrared Diffuse Reflection Spectroscopy

WANG Xiao-liang, ZHANG Bing-hua, FENG Run-dong, ZHONG Hong-mei, Xi Zhi-fang   

  1. Shanxi Institute for Food and Drug Control, Shaanxi Xi'an 710065, China
  • Received:2015-09-01 Revised:2015-09-01 Online:2015-07-08 Published:2015-09-02

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190

摘要： 目的 利用近红外漫反射光谱分析技术和化学计量学方法对硝酸咪康唑栓剂进行快速定量分析。方法 以9个厂家生产的42批硝酸咪康唑栓剂分析对象,首先采集样品的近红外漫反射光谱,并以法定方法测定其含量,最后采用偏最小二乘法建立定量模型。结果 采用内部交叉验证建立模型。含量范围为7.21%~19.92%;建模谱段为9 994~4 551 cm-1;预处理方法为一阶导结合矢量归一化,13点平滑;维数为7;内部交叉验证相关系数为96.674%;均方根误差分别为0.509%。结论 所建立的释放度快速分析定量模型可对硝酸咪康唑栓剂进行准确、快速定量分析,方法快速简便,可用于药品的快速分析和检验。

关键词: 硝酸咪康唑栓, 近红外光谱, 快速定量分析, 化学计量

Abstract: Objective To quantitatively analyze the miconazole nitrate suppository by near infrared diffuse reflection spectroscopy technology and chemometrics. Methods 42 batches of miconazole nitrate suppositories from 9 different manufacturers were chosen for analyzing. Firstly, collected the near infrared diffuse reflection spectrum of the samples. Secondly, determined the active pharmaceutical ingredient (API) contents by conventional method. Thirdly, developed the model with the partial least square (PLS) algorithm available in the Quant 2. Results Our model was based on cross validation with API from 7.21% to 19.92% in calibration set. The spectra ranges were 9 994~4 551 cm-1; the pretreatment method was first derivation and vector normalization with smooth points 13; the rank was 7. In the cross validation, the values of R2 and RMSECV were 96.674.04% and 0.50% (mg·mg-1), respectively. Conclusion The method is accurate, quick and convenient, which can be used for quick analysis in drug control.

Key words: miconazole nitrate suppository, near infrared spectroscopy, quick quantitative analysis, chemometrics

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