基于PXRD、DSC和NIR技术的那格列奈多晶型的定量分析方法研究(英文)

第39卷第4期 2016年12月

南京师大学报（自然科学版）

JOURNAL OF NANJING NORMAL UNIVERSITY( Natural Science Edition)

Vol. 39 No. 4

Dec,2016

doi：10.3969/j.issn.l001-4616.2016.04.013

A Comparative Study on Quantification of Binary Polymorphic Mixtures of Nateglinide by Using Powder X-Ray Diffraction,Differential Scanning Calorimetry and Near Infrared Spectroscopy

Qiu Jingbo,Xie Mengyu,Shen Xiaomin,Zhou Dan,Zhu Murong,Li Gang (School of Life Sciences,Testing & Analysis Center,Nanjing Normal University,Nanjing 210023 ,China)

A bstract：The aim of this study is to evaluate the ability of powder X-ray diffraction(PXRD) differential scanning calo-

rimetry ( DSC) and near infrared( NIR) spectroscopy to quantify two polymorphic form s(B,H)of nateglinide in binary powder mixtures. For this purpose, univariate and multivariate method are developed. The results show that PXRD (with PLS regression) provides a reliable determination of nateglinide samples( predicted accuracy of 89.1% ) ,which is the best choice for quantification of nateglinide polymorphic mixtures in practice, while NIR spectroscopy is the least accurate (predicted accuracy of 79.6%) mainly due to the effect of sample inhomogeneity. Though a good linear relation and a high predicted accuracy(93.4%)for DSC are successfully obtained,it could not be a practical way for low-content quanti-fication in nateglinide polymorphic mixtures.

Key words ： nateglinide polymorphs, quantification, powder X-ray diffraction, differential scanning calorimetry, near infra-red spectroscopy

CLC num ber：R917 Document code：A Article ID：1001-4616(2016)04-0071-11

基于PXRD、D S C和N IR技术的那格列奈多晶型的定量分析方法研究

邱晶波，谢梦雨，沈晓敏，周丹，朱慕荣，李钢

(南京师范大学生命科学学院,分析测试中心，江苏南京21〇〇23)

[摘要]从晶体学、热力学和光谱学三个角度展开对那格列奈多晶型的定量分析研究，通过X-射线粉末衍射法、差示扫描量热法及近红外光谱分析技术，并结合化学计量学的方法，建立了那格列奈B晶型和H晶型二元 混合体系的定量分析模型.结果表明，近红外光谱法虽然操作简单快速，但模型的预测准确率和方法的灵敏度较低;差示扫描量热法虽然准确度较高，但实用性较差;利用PXRD结合PL S法得到的结果最好，模型比较稳定，不易受样品的影响，可用于实际工作中.为那格列奈制剂产品及其他多晶型药物的定量分析奠定了理论基础.

[关键词]那格列奈多晶型，定量分析，X-射线粉末衍射法，差示扫描量热法，近红外光谱法

P olym orp hism is a w e ll recognized phenom enon ,i.e. a solid m a te ria l e xistin g in two o r more c ry s ta llin e pha-ses w ith d iffe re n t arrangem ents o r conform ations in the crystal la ttic e^1. D ru g polym orphs are d iffe re n t c rys ta l-lin e form s o f the same d ru g substance. I t has been estim ated that more than h a lf o f active p h a rm a ceutica l in g re d i- e n ts( A P Is) exist in m ore than one p o lym o rp h ic form. D iffe re n t A P I polym orphs have d iffe re n t p h ysica l and chem-ic a l p ro p e rtie s, thus causing changes in the s o lu b ility, s ta b ility, d is s o lu tio n, b io a v a ila b ility, and fin a l e ffica cy o f drugs ^3The string en t regulatory constraints forces pharm a ceutica l com panies to deal w ith po lym o rp hism o f Received data；2016-07-24.

Foundation item ：Supported by Jiangsu Large Scientific Instruments Shared Services Platform Foundation ( BZ201403). Corresponding author：Li Gang,professor,majored in XRD analysis. E-mail：ligangl@ https://www.wendangku.net/doc/7116116736.html,

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