Walash Mohamed, Belal Fathalla, Eid Manal, el-Abass Samah Abo
Department of Analytical Chemistry, Faculty of Pharmacy, Mansoura University, Mansoura, 35516, Egypt.
J Chromatogr Sci. 2011 Feb;49(2):159-64. doi: 10.1093/chrsci/49.2.159.
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.
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。
