化学分析计量
化學分析計量
화학분석계량
CHEMICAL ANALYSIS AND METERAGE
2013年
5期
37-40
,共4页
高效液相色谱法%衍生化%加巴喷丁%对甲氧基苯磺酰氯
高效液相色譜法%衍生化%加巴噴丁%對甲氧基苯磺酰氯
고효액상색보법%연생화%가파분정%대갑양기분광선록
high performance liquid chromatography%derivatization%gabapentin%4-Methoxybenzenesulfonyl chloride
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30 min。以0.05 mol/L Na2HPO4缓冲液(pH 10.0)-甲醇混合液为流动相,分析柱为反相ODS柱(150 mm×4.6 mm,5μm),柱温为室温,流速为0.8 mL/min,检测波长为240 nm。加巴喷丁溶液质量浓度在1~100 mg/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。
採用紫外衍生劑對甲氧基苯磺酰氯(MOBS-Cl)對加巴噴丁進行衍生反應,建立瞭一種柱前衍生測定加巴噴丁的新方法。最佳衍生化條件:對甲氧基苯磺酰氯與加巴噴丁的質量比大于7.5∶1,于50℃水浴中反應30 min。以0.05 mol/L Na2HPO4緩遲液(pH 10.0)-甲醇混閤液為流動相,分析柱為反相ODS柱(150 mm×4.6 mm,5μm),柱溫為室溫,流速為0.8 mL/min,檢測波長為240 nm。加巴噴丁溶液質量濃度在1~100 mg/L範圍內與色譜峰麵積線性關繫良好,線性方程為A=24.5667c+12.3025,相關繫數r=0.9999,測定結果的相對標準偏差(RSD)為0.56%,加巴噴丁的檢測下限為0.017μg/g。
채용자외연생제대갑양기분광선록(MOBS-Cl)대가파분정진행연생반응,건립료일충주전연생측정가파분정적신방법。최가연생화조건:대갑양기분광선록여가파분정적질량비대우7.5∶1,우50℃수욕중반응30 min。이0.05 mol/L Na2HPO4완충액(pH 10.0)-갑순혼합액위류동상,분석주위반상ODS주(150 mm×4.6 mm,5μm),주온위실온,류속위0.8 mL/min,검측파장위240 nm。가파분정용액질량농도재1~100 mg/L범위내여색보봉면적선성관계량호,선성방정위A=24.5667c+12.3025,상관계수r=0.9999,측정결과적상대표준편차(RSD)위0.56%,가파분정적검측하한위0.017μg/g。
A new UV-derived agents 4-Methoxybenzenesulfonyl chloride(MOBS-Cl)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,5μm)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 0.017μg/g.