水解法与超声法检测保健品中支链氨基酸粉的支链氨基酸比对

Comparison of determination of branched chain amino acids in branched chain amino acid powders in health products by hydrolysis method and ultrasound method

中文关键词:  保健食品  支链氨基酸  水解法  超声法  前处理

英文关键词:health food  branched chain amino acids  hydrolysis method  ultrasonic method  pretreatment

中文摘要:

      目的 比较水解法与超声法测定保健品中支链氨基酸粉的支链氨基酸(亮氨酸、异亮氨酸及缬氨酸)含量的分析方法。 方法 样品分别经水解法和超声法进行前处理后, 经Agilent Eclipse XDB-phenyl柱分离, 以甲醇和0.1%甲酸溶液为流动相, 梯度洗脱, 流速为0.4 mL/min, 柱温40 ℃, 采用液相色谱-质谱法检测。结果 亮氨酸、异亮氨酸及缬氨酸在0.01~0.05 mmol/L的浓度范围内, 线性关系良好, 相关系数r均大于0.99。样品经2种方法处理后, 都能够准确检测支链氨基酸的含量, 2种方法的实验结果比对的相对误差均<5%, 水解法处理的精密度相对标准偏差为4.0%~5.3%, 而超声方法的精密度相对标准偏差均小于5.0%。结论 与水解法相比, 超声法前处理方法操作简便, 分离效果明显, 更适用于提取保健食品中支链氨基酸粉。

英文摘要:

      Objective To compare the determination of branched chain amino acids in branched chain amino acid powders in health products by hydrolysis method and ultrasound method. Methods The samples were pretreated by hydrolysis and ultrasound, respectively, and then separated with Agilent Eclipse xdb-phenyl column at the flow rate of 0.4 mL/min by gradient elution using methanol and 0.1% formic acid as the mobile phase, and the temperature of the column oven was maintained at 40 ℃. The sample was determined by liquid chromatography-mass spectrometry. Results Leucine, isoleucine and valine had a good linear relationship within the concentration range of 0.01-0.05 mmol/L, and the correlation coefficient was all greater than 0.99. After being treated by 2 methods, the branched chain amino acids content of all samples could be accurately detected. The relative error of the comparison of the experimental results of the two methods was <5%, the relative standard deviations of precision treated by the hydrolysis method were 4.0%-5.3%, and the relative standard deviations of precision treated by the ultrasonic method were less than 5.0%. Conclusion Compared with hydrolysis method, the ultrasonic pre-process is simple, effective and more suitable to extract branched chain amino acid powder from health food.