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采用 HPLC 法同时测定药物制剂及尿样中的一些抗抑郁药和维生素 B。

Simultaneous determination of some antidepressant drugs and vitamin B in pharmaceutical products and urine sample using HPLC method.

机构信息

Chemistry Department, Faculty of Science, Cairo University, Giza 12613, Egypt; Egypt Nanotechnology Center, Cairo University, El-Sheikh Zayed, 6th October, Giza, 12588, Egypt.

Chemistry Department, Faculty of Science, Cairo University, Giza 12613, Egypt.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2020 Aug 1;1150:122178. doi: 10.1016/j.jchromb.2020.122178. Epub 2020 May 19.

Abstract

Three sensitive, accurate and precise HPLC methods were devolved for the simultaneous determination of vilazodone HCl (VILHC), agomelatine (AGO) or duloxetine HCl (DULHC) and vitamin B (cyanocoblamine B) in bulk, pharmaceutical dosage form and in urine samples. Both similar methods (I and II) were carried out using 0.04 M phosphate buffer (pH 7.0), acetonitrile and methanol in the ratio (30:30:40, v/v) as a mobile phase. Thermo BDS hypersil-C18 column, with 5 μm particle size and 250 × 4.5 mm dimensions, at flow rate 1.0 mL min and UV detection at 277 nm at ambient temperature 25 °C were used. The retention times were 5.12 and 2.54 min for VILHC and vitamin B, 4.98 and 2.53 min for AGO and vitamin B, respectively, with linearity range from 0.001 to 200 μg mL. However, for the separation of DULHC and B, UV detection at 230 nm and Agilent Eclipse XDA-C8 (150 × 4.5 mm, 5 μm) column, were used (method III). The retention time of DULHC and vitamin B was found to be 4.53 and 1.35 min, respectively, with linearity range from 0.0005 to 200 μg mL. The proposed methods were validated as per the ICH guideline with very low LOD and LOQ. The values of %RSD for precision was less than 2% and the value of % recovery were found to be 99.20-100.9% and 99.23-100.67% for determination of the drugs in pure and pharmaceutical formulations, respectively, for all methods confirming that the methods are precise, accurate and selective for separation and determination of VILHC, AGO or DULHC from B in tablets and in urine samples without any interference from each other or from common excipients.

摘要

三种灵敏、准确、精密的 HPLC 方法被开发出来,用于同时测定盐酸维拉佐酮(VILHC)、阿戈美拉汀(AGO)或盐酸度洛西汀(DULHC)和维生素 B(氰钴胺素 B)的原料药、制剂和尿液样品。两种相似的方法(I 和 II)均使用 0.04 M 磷酸盐缓冲液(pH 7.0)、乙腈和甲醇,比例为(30:30:40,v/v)作为流动相。Thermo BDS Hypersil-C18 柱,粒径 5μm,250×4.5mm 尺寸,流速 1.0mL/min,277nm 处 UV 检测,在 25°C 环境温度下使用。VILHC 和维生素 B 的保留时间分别为 5.12 和 2.54min,AGO 和维生素 B 的保留时间分别为 4.98 和 2.53min,线性范围为 0.001-200μg/mL。然而,对于 DULHC 和 B 的分离,使用 230nm 的 UV 检测和 Agilent Eclipse XDA-C8(150×4.5mm,5μm)柱(方法 III)。DULHC 和维生素 B 的保留时间分别为 4.53 和 1.35min,线性范围为 0.0005-200μg/mL。所提出的方法按照 ICH 指南进行了验证,具有非常低的 LOD 和 LOQ。精密度的 %RSD 值小于 2%,三种方法在纯品和制剂中测定药物的回收率分别为 99.20-100.9%和 99.23-100.67%,这表明这些方法对于从片剂和尿液样品中分离和测定 VILHC、AGO 或 DULHC 与 B 是精确、准确和选择性的,彼此之间或与常见赋形剂之间没有任何干扰。

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