CAJ | 학술논문

利用2,4-二硝基氟苯为柱前衍生剂,建立了用高效液相色谱法测定普瑞巴林的方法.考察了光、反应温度、摩尔比和反应时间对衍生化反应的影响,确定了最佳衍生反应条件:在65℃水浴中避光反应75 min.色谱柱为C_(18),流动相为50 mmol·L~(-1) KH_2PO_4(pH = 3.0)/乙腈(30/70,v/v),检测波长为360 nm,流速为1.0 mL·min~(-1),柱温为35℃.实验结果:在8～48 μg·mL~(-1)范围内呈较好的线性关系(r=0.9998),回收率(100.03±1.10)%(n=9),不同浓度下日内精密度0.82%、0.77%和1.87%,8h内稳定性良好(RSD = 1.92%),检测限低至0.8 ng·mL~(-1).实验表明该方法简便、快速、准确、灵敏.通过对该方法的实际应用,三批样品测定值的RSD分别为0.59%、0.68%和1.04%,表明该方法能够用于测定普瑞巴林的含量.
이용2,4-이초기불분위주전연생제,건립료용고효액상색보법측정보서파림적방법.고찰료광、반응온도、마이비화반응시간대연생화반응적영향,학정료최가연생반응조건:재65℃수욕중피광반응75 min.색보주위C_(18),류동상위50 mmol·L~(-1) KH_2PO_4(pH = 3.0)/을정(30/70,v/v),검측파장위360 nm,류속위1.0 mL·min~(-1),주온위35℃.실험결과:재8～48 μg·mL~(-1)범위내정교호적선성관계(r=0.9998),회수솔(100.03±1.10)%(n=9),불동농도하일내정밀도0.82%、0.77%화1.87%,8h내은정성량호(RSD = 1.92%),검측한저지0.8 ng·mL~(-1).실험표명해방법간편、쾌속、준학、령민.통과대해방법적실제응용,삼비양품측정치적RSD분별위0.59%、0.68%화1.04%,표명해방법능구용우측정보서파림적함량.
A high performance liquid chromatographic (HPLC) method with UV detection was developed to determine the content of Pregabalin (PGB) by using 1-fluoro-2,4-dinitrobenzene (DNFB) as the precolumn derivatization reagent. The effects of light, reaction temperature, molar ratio of DNFB to PGB and reaction time on the derivatization reaction were investigated. Chromatographic separation was achieved on a C_(18) column with a mixture of phosphate buffer and acetonitrile as the mobile phase. The relationship between the PGB concentration and the PGB-DNFB peak area on the chromatograph is linear over the PGB concentration range of 8～48 μg·mL~(-1) (r = 0.9998). The recover ratio is (100.03 ± 1.10)% (n = 9). The within-day precisions are 0.82%, 0.77% and 1.87% for three different PGB concentrations (n = 6), respectively. The derivative solution is stable within 8 hours (RSD = 1.92%). The LOD is as low as 0.8 ng·mL~(-1). The proposed PGB content determination method is simple, rapid, accurate and reliable.