[目的]建立“染红食品”中苏丹红Ⅰ、Ⅱ、Ⅲ和Ⅳ残留量的高效液相色谱(HPLC)初筛、质谱确认分析方法。[方法]以Merck RP-18柱为分析柱,流动相:乙腈∶水=90∶10,Waters-2996二极管矩阵检测器(PDA)和FinniganLCQ Deca XP MAX质谱仪为检测...[目的]建立“染红食品”中苏丹红Ⅰ、Ⅱ、Ⅲ和Ⅳ残留量的高效液相色谱(HPLC)初筛、质谱确认分析方法。[方法]以Merck RP-18柱为分析柱,流动相:乙腈∶水=90∶10,Waters-2996二极管矩阵检测器(PDA)和FinniganLCQ Deca XP MAX质谱仪为检测器。[结果]回归方程和相关系数为:苏丹红Ⅰ:y=0.163104x+0.019217,r=0.99993;苏丹红Ⅱ:y=0.153674x-0.2212981,r=0.99993;苏丹红Ⅲ:y=0.305919x-5.0810264,r=0.9997;苏丹红Ⅳ:y=0.239273x-5.260669,r=0.9997。平均回收率(%):87.3、83.0、86.7和90.0。[结论]用HPLC-PDA-MS法检测食品中的苏丹红方法简便,重现性好,灵敏度高,定性准确,定量精确。展开更多
Drug stability is closely related to drug safety and needs to be considered in the process of drug production,package and storage.To investigate the stability of epalrestat,a carboxylic acid derivative,a reversed-phas...Drug stability is closely related to drug safety and needs to be considered in the process of drug production,package and storage.To investigate the stability of epalrestat,a carboxylic acid derivative,a reversed-phase high-performance liquid chromatography(RP-HPLC)method was developed in this study and applied to analyzing the degradation kinetics of epalrestat in aqueous solutions in various conditions,such as different pH,temperatures,ionic strengths,oxidation and irradiation.The calibration curve was A=1.6×10^5C–1.3×10^3(r=0.999)with the liner range of 0.5–24μg/mL,the intra-day and inter-day precision was less than 2.0%,as was the repeatibility.The average accuracy for different concentrations was more than 98.5%,indicating that perfect recoveries were achieved.Degradation kinetic parameters such as degradation rate constants(k),activation energy(Ea)and shelf life(t0.9)under different conditions were calculated and discussed.The results indicated that the degradation behavior of epalrestat was pH-dependent and the stability of epalrestat decreased with the rised irradiation and ionic strength;however,it was more stable in neutral and alkaline conditions as well as lower temperatures.The results showed that the degradation kinetics of epalrestat followed first-order reaction kinetics.Furthermore,the degradation products of epalrestat under stress conditions were identified by UHPLC-PDA-MS/MS,with seven degradation products being detected and four of them being tentatively identified.展开更多
文摘[目的]建立“染红食品”中苏丹红Ⅰ、Ⅱ、Ⅲ和Ⅳ残留量的高效液相色谱(HPLC)初筛、质谱确认分析方法。[方法]以Merck RP-18柱为分析柱,流动相:乙腈∶水=90∶10,Waters-2996二极管矩阵检测器(PDA)和FinniganLCQ Deca XP MAX质谱仪为检测器。[结果]回归方程和相关系数为:苏丹红Ⅰ:y=0.163104x+0.019217,r=0.99993;苏丹红Ⅱ:y=0.153674x-0.2212981,r=0.99993;苏丹红Ⅲ:y=0.305919x-5.0810264,r=0.9997;苏丹红Ⅳ:y=0.239273x-5.260669,r=0.9997。平均回收率(%):87.3、83.0、86.7和90.0。[结论]用HPLC-PDA-MS法检测食品中的苏丹红方法简便,重现性好,灵敏度高,定性准确,定量精确。
文摘Drug stability is closely related to drug safety and needs to be considered in the process of drug production,package and storage.To investigate the stability of epalrestat,a carboxylic acid derivative,a reversed-phase high-performance liquid chromatography(RP-HPLC)method was developed in this study and applied to analyzing the degradation kinetics of epalrestat in aqueous solutions in various conditions,such as different pH,temperatures,ionic strengths,oxidation and irradiation.The calibration curve was A=1.6×10^5C–1.3×10^3(r=0.999)with the liner range of 0.5–24μg/mL,the intra-day and inter-day precision was less than 2.0%,as was the repeatibility.The average accuracy for different concentrations was more than 98.5%,indicating that perfect recoveries were achieved.Degradation kinetic parameters such as degradation rate constants(k),activation energy(Ea)and shelf life(t0.9)under different conditions were calculated and discussed.The results indicated that the degradation behavior of epalrestat was pH-dependent and the stability of epalrestat decreased with the rised irradiation and ionic strength;however,it was more stable in neutral and alkaline conditions as well as lower temperatures.The results showed that the degradation kinetics of epalrestat followed first-order reaction kinetics.Furthermore,the degradation products of epalrestat under stress conditions were identified by UHPLC-PDA-MS/MS,with seven degradation products being detected and four of them being tentatively identified.
基金supported by the Agricultural Research Service of the U.S. Department of Agriculture and an Interagency Agreement with the Office of Dietary Supplements of the National Institutes of Health
