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同时测定复方片剂中卡格列净和二甲双胍的比较液相色谱研究

Comparative Liquid Chromatographic Study for Concurrent Determination of Canagliflozin and Metformin in Combined Tablets.

作者信息

Zaghary Wafaa A, Mowaka Shereen, Hendy Moataz S

机构信息

Pharmaceutical Chemistry Department, Faculty of Pharmacy, Helwan University, Ein Helwan, Cairo 11795, Egypt.

Pharmaceutical Chemistry Department, Faculty of Pharmacy, The British University in Egypt, El-Sherouk City, Cairo 11837, Egypt.

出版信息

J Anal Methods Chem. 2017;2017:9197230. doi: 10.1155/2017/9197230. Epub 2017 Dec 3.

Abstract

New HPLC-UV method (method A), for simultaneous determination of metformin (MET) and canagliflozin (CANA), was developed and compared to another novel UPLC-UV method (method B) in their tablet combination. Concerning method A, isocratic separation was done by C18 column (100 mm × 2.1 mm, 3 m) using methanol and 0.03 M phosphate buffer (75 : 25, /) at pH 3.2 as a mobile phase. Meanwhile, chromatographic separation in method B was achieved via Hypersil® gold (50 mm × 2.1 mm, 1.9 m). Mobile phase was methanol and 0.03 M phosphate buffer at ratio of 80 : 20  /. In both, detection was done at wavelength of 240 nm. Method A showed satisfactory linearity results over 1-50 g·mL and 0.5-100 g·mL, while method B linearity was at 0.1-50 g·mL and 0.25-100 g·mL for CANA and MET, respectively. In terms of accuracy and precision, method A accuracy was 99.81 ± 0.73 and 99.37 ± 0.54, while method B gave accuracy of 99.47 ± 1.03 and 99.73 ± 0.89 for CANA and MET, respectively. For precision, the % RSD was found to be less than 2% for three concentrations analyzed three times. The two methods are convenient for quality laboratories, yet the UPLC method offered the advantage of shorter run times and higher sensitivity.

摘要

开发了一种用于同时测定二甲双胍(MET)和卡格列净(CANA)的新型高效液相色谱 - 紫外法(方法A),并将其与另一种新型超高效液相色谱 - 紫外法(方法B)用于其片剂组合分析时进行比较。关于方法A,采用C18柱(100 mm×2.1 mm,3μm),以甲醇和0.03 M磷酸盐缓冲液(75 : 25,v/v)在pH 3.2作为流动相进行等度分离。同时,方法B的色谱分离通过Hypersil® gold柱(50 mm×2.1 mm,1.9μm)实现。流动相为甲醇和0.03 M磷酸盐缓冲液,比例为80 : 20(v/v)。两种方法均在240 nm波长处进行检测。方法A在1 - 50μg·mL和0.5 - 100μg·mL范围内显示出令人满意的线性结果,而方法B对于CANA和MET的线性范围分别为0.1 - 50μg·mL和0.25 - 100μg·mL。在准确度和精密度方面,方法A的准确度分别为99.81±0.73和99.37±0.54,而方法B对于CANA和MET的准确度分别为99.47±1.03和99.73±0.89。对于精密度,对三种浓度进行三次分析时,相对标准偏差(%RSD)均小于2%。这两种方法对质量控制实验室都很方便,但超高效液相色谱法具有运行时间短和灵敏度高的优点。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5958/5733124/507cadbb21a3/JAMC2017-9197230.001.jpg

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