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同时用高效液相色谱法测定秋水仙碱硫代糖苷与格拉非宁以及秋水仙碱硫代糖苷与氟硝丁酰胺在其复方制剂中的含量。

Simultaneous HPLC determination of thiocolchicoside and glafenine as well as thiocolchicoside and floctafenine in their combined dosage forms.

作者信息

Walash Mohamed, Belal Fathalla, Eid Manal, el-Abass Samah Abo

机构信息

Department of Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura, 35516, Egypt.

出版信息

J Chromatogr Sci. 2011 Feb;49(2):159-64. doi: 10.1093/chrsci/49.2.159.

Abstract

Sensitive and accurate high-performance liquid chromatographic methods have been developed for the simultaneous determination of thiocolchicoside (TC)-glafenine (GF) (Mix I) and thiocolchicoside-floctafenine (FN) (Mix II) in their pharmaceutical formulations. The analysis for both mixtures was performed using 250 mm × 4.6 mm i.d., 5 μm particle size C18 Waters Symmetry column. The mobile phase consisted of methanol-0.035 M phosphate buffer (50:50, v/v) of pH 4.5 for Mix I and methanol-0.03 M phosphate buffer (70:30, v/v) of pH 4 for Mix II with flow rate of 1 mL/min and UV detection at 400 nm in both cases. The calibration plots were rectilinear over the concentration range of 0.2-2 μg/mL for TC in both mixtures and 20-200 μg/mL for each of GF and FN . The limits of detection for TC and GF were 0.05 μg/mL and 0.62 μg/mL, respectively, and for TC and FN were 0.02 μg/mL and 0.70 μg/mL, respectively. Additionally, the proposed methods were successfully applied to their combined tablets with average percentage recoveries of 100.35 ± 0.61 and 100.57 ± 0.72% for TC and GF respectively and for TC and FN the percentage recoveries were 101.2 ± 0.72 and 100.36 ± 0.67%, respectively. The results obtained were favorably compared with those given using the comparison methods.

摘要

已开发出灵敏且准确的高效液相色谱法,用于同时测定其药物制剂中的硫代秋水仙碱(TC)-格拉非宁(GF)(混合物I)和硫代秋水仙碱-氟洛芬(FN)(混合物II)。两种混合物的分析均使用内径为250 mm×4.6 mm、粒径为5 μm的沃特世Symmetry C18柱。混合物I的流动相为甲醇-0.035 M磷酸盐缓冲液(50:50,v/v),pH值为4.5;混合物II的流动相为甲醇-0.03 M磷酸盐缓冲液(70:30,v/v),pH值为4,两种情况下流速均为1 mL/min,紫外检测波长均为400 nm。两种混合物中TC的校准曲线在0.2 - 2 μg/mL浓度范围内呈线性,GF和FN各自的校准曲线在20 - 200 μg/mL浓度范围内呈线性。TC和GF的检测限分别为0.05 μg/mL和0.62 μg/mL,TC和FN的检测限分别为0.02 μg/mL和0.70 μg/mL。此外,所提出的方法成功应用于它们的复方片剂,TC和GF的平均回收率分别为100.35±0.61%和100.57±0.72%,TC和FN的回收率分别为101.2±0.72%和100.36±0.67%。所得结果与使用对照方法得到的结果相比具有优势。

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