柱前衍生高效液相色谱法检测加巴喷丁衍生化条件的研究

Precolumn Derivatization Optimization about Determination of Gabapentin by High Performance Liquid Chromatography

采用紫外衍生剂对甲氧基苯磺酰氯（MOBS-Cl）对加巴喷丁进行衍生反应，建立了一种柱前衍生测定加巴喷丁的新方法。最佳衍生化条件：对甲氧基苯磺酰氯与加巴喷丁的质量比大于7．5-1，于50℃水浴中反应30min。以0．05mol／LNa2HPO4缓冲液（pH10．0）-甲醇混合液为流动相，分析柱为反相ODS柱（150mm×4．6mm，5μm），柱温为室温．流速为0．8mL／min，检测波长为240rim。加巴喷丁溶液质量浓度在1-100mg／L范围内与色谱峰面积线性关系良好，线性方程为A=24．5667c＋12．3025，相关系数r=0．9999，测定结果的相对标准偏差（RSD）为0．56％，加巴喷丁的检测下限为0．017μg／g。

A new UV-derived agents 4-Methoxybenzenesulfonyl chloride （ MOBS-C1 ） of gabapentin was used to establish a method to determine gabapentin by a pre-column derivatization. The best conditions were： the mass ratio of 4-Methoxybenzenesulfonyl chloride and gabapentin was greater than 7.5 ： 1, the reaction lasted for 30 min at 50℃ （ water bath ）. 0.05 mol / L Na2HPO4 buffer （ pH 10.0 ）-methanol was as the mobile phase, reversed-phase ODS column （ 150 mm × 4.6 mm, 5 μ m ） as the analytical column, column temperature at room temperature with the flow rate of 0.8 mL / min and detection wavelength of 240 nm, the chromatography peak area was linear relationship with the mass concent in the range of 1-100 mg/L, the linear equation was A=24.566 7c （ mg/L ） ＋12.302 5, r=0.999 9, the relative standard deviation was 0.56%, the detection limit was 0.017 μg/g.