CAJ | 학술논문

目的：应用蒸发光散射检测器（evaporative light scattering detector, ELSD）、“HALO”核-壳型新型填料液相色谱柱，建立一种高效液相色谱-蒸发光散射检测法（HPLC-ELSD）直接测定20种未衍生氨基酸的分析方法，并将其用于复方氨基酸注射液中氨基酸含量的测定。方法：采用核-壳型HALO色谱柱（4.6 mm×150 mm，2.7mm C18），以甲醇-九氟戊酸-七氟丁酸-三氟乙酸-水为流动相进行梯度洗脱，流速0.5 ml/min，ELSD飘移管温度40℃，载气流速3.0 L/min，对20种基本氨基酸进行分离检测。结果：氨基酸的质量浓度在0.01～1.0 mg/ml范围内，其峰面积的对数值与进样质量的对数值呈良好的线性关系；氨基酸的检出限介于20～50 ng之间，样品加标回收率为89.0％～111.2％。结论：该方法操作简便快速、准确可靠，溶剂消耗少，为药品、食品、饲料及化工生产等领域混合氨基酸样品的直接检测提供了参考。
목적：응용증발광산사검측기（evaporative light scattering detector, ELSD）、“HALO”핵-각형신형전료액상색보주，건립일충고효액상색보-증발광산사검측법（HPLC-ELSD）직접측정20충미연생안기산적분석방법，병장기용우복방안기산주사액중안기산함량적측정。방법：채용핵-각형HALO색보주（4.6 mm×150 mm，2.7mm C18），이갑순-구불무산-칠불정산-삼불을산-수위류동상진행제도세탈，류속0.5 ml/min，ELSD표이관온도40℃，재기류속3.0 L/min，대20충기본안기산진행분리검측。결과：안기산적질량농도재0.01～1.0 mg/ml범위내，기봉면적적대수치여진양질량적대수치정량호적선성관계；안기산적검출한개우20～50 ng지간，양품가표회수솔위89.0％～111.2％。결론：해방법조작간편쾌속、준학가고，용제소모소，위약품、식품、사료급화공생산등영역혼합안기산양품적직접검측제공료삼고。
Objective:An analytical method for the determination of 20 underivatized amino acids was established using HPLC with HALO column coupled with an evaporative light-scattering detector (ELSD).Methods:The HALO column was packed with a core-shell C18 stationary phase (4.6 mm×150 mm, 2.7mm). A solvent gradient elution was performed with nonalfuoropentanoic acid-heptalfuorobutyric acid containing trilfuoroacetic acid as mobile phase A and methanol as mobile phase B. The temperature of the drift tube in ELSD was set at 40℃ and the lfow rate of carrier gas was 3.0 L/min.Results:There was a good linear relationship between the logarithm of the peak area and logarithm of the mass of each separated amino acid. The limits of detection for the underivatized amino acids were from 20 ng to 50 ng. The average recoveries of the 20 amino acids were between 89.0%and 111.2%.Conclusion: This method is simple, rapid and accurate for the determination of underivatized amino acids and can be widely used for the determination of underivatized amino acids in pharmaceutical, food, animal feeds and chemical industries.