Walash Mohamed I, Kh Sharaf El-Din Mohie M, El-Enany Nahed M, Eid Manal I, Shalan Shereen M
Department of Analytical Chemistry, Faculty of Pharmacy, University of Mansoura, Mansoura, 35516, Egypt.
Chem Cent J. 2012 Feb 14;6:13. doi: 10.1186/1752-153X-6-13.
A new simple, rapid and sensitive reversed-phase liquid chromatographic method was developed and validated for the simultaneous determination of sulpiride (SUL) and mebeverine Hydrochloride (MEB) in the presence of their impurities and degradation products. The separation of these compounds was achieved within 6 min on a 250 mm, 4.6 mm i.d., 5 m particle size Waters®-C18 column using isocractic mobile phase containing a mixture of acetonitrile and 0.01 M dihydrogenphosphate buffer (45:55) at pH = 4.0. The analysis was performed at a flow rate of 1.0 mL/min with fluorescence-detection at excitation 300 nm and emission at 365 nm. The concentration-response relationship was linear over a concentration range of 10- 100 ng/mL for both MEB and SUL with a limit of detection 0.73 ng/mL and 0.85 ng/mL for MEB and SUL respectively. The proposed method was successfully applied for the analysis of both MEB and SUL in bulk with average recoveries of 100.22 ± 0.757% and 99.96 ± 0.625% respectively, and in commercial tablets with average recoveries of 100.04 ± 0.93% and 100.03 ± 0.376% for MEB and SUL respectively. The proposed method was successfully applied to the determination of MEB metabolite (veratic acid) in real plasma simultaneously with SUL. The mean% recoveries (n = 3) for both MEB metabolite (veratic acid) and SUL were 100.36 ± 2.92 and 99.06 ± 2.11 for spiked human plasma respectively. For real human plasma, the mean% recoveries (n = 3) were and respectively.
建立并验证了一种新的简单、快速且灵敏的反相液相色谱法，用于同时测定舒必利（SUL）和盐酸美贝维林（MEB）及其杂质和降解产物。在一根250 mm×4.6 mm内径、5 µm粒径的沃特世®-C18柱上，使用含乙腈和0.01 M磷酸二氢盐缓冲液（45:55）、pH = 4.0的等度流动相，在6分钟内实现了这些化合物的分离。分析在流速为1.0 mL/min下进行，采用荧光检测，激发波长为300 nm，发射波长为365 nm。MEB和SUL在10 - 100 ng/mL的浓度范围内浓度-响应关系呈线性，MEB和SUL的检测限分别为0.73 ng/mL和0.85 ng/mL。所提出的方法成功应用于MEB和SUL原料药的分析，平均回收率分别为100.22±0.757%和99.96±0.625%，在市售片剂中的平均回收率分别为100.04±0.93%和100.03±0.376%。所提出的方法成功应用于同时测定实际血浆中MEB的代谢物（藜芦酸）和SUL。对于加标的人血浆，MEB代谢物（藜芦酸）和SUL的平均回收率（n = 3）分别为100.36±2.92和99.06±2.11。对于实际人血浆，平均回收率（n = 3）分别为……和……（原文此处未给出具体数据） 。
