超高效液相色谱-串联质谱法测定酸笋中多种游离氨基酸含量

目的 建立超高效液相色谱-串联质谱法测定柳州螺蛳粉原料酸笋中苯丙氨酸、亮氨酸、异亮氨酸等16种游离氨基酸含量的方法。方法 匀浆后的样品用水作为溶剂超声提取、离心过滤后,采用BEHAmide色谱柱分离,经甲酸铵水溶液-乙腈体系梯度洗脱,超高效液相色谱-串联质谱仪以正离子扫描,多反应监测模式进行检测。结果 建立的测定方法对各氨基酸分离效果及峰型良好,在0.5～10.0μg/mL线性范围内,相关系数(r)均大于0.998, 16种氨基酸在各自质量浓度范围内均呈现良好线性关系,方法检出限0.23～4.59 mg/kg。样品在3个添加水平(25、50、100 mg/kg)的平均加标回收率为78.1%～114.4%,相对标准偏差0.7%～6.6%。测定部分预包装柳州螺蛳粉生产厂采样的酸笋原料,各氨基酸含量为0～625.8 mg/kg。结论 该方法简便快捷、测定高效,可用于酸笋的多种氨基酸含量分析测定。

Determination of multiple free amino acids in fermented bamboo shoots by ultra performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for the determination the 16 kinds of free amino acids such as phenylalanine,leucine and isoleucine in fermented bamboo shoots of Liuzhou river snails rice noodle by ultra performance liquid chromatography-tandem mass spectrometry.Methods After homogenization,the samples were extracted by ultrasonic extraction with water as solvent,filtered by centrifugation,and separated by BEH Amide column.The samples were eluted by gradient elution of ammonium formate aqueous solution and acetonitrile system,and detected by ultra performance liquid chromatography-tandem mass spectrometry with positive ion scanning and multiple reaction monitoring.Results The established determination method in this experiment showed good separation and shape of peak for each amino acid,good linear relationships in the range of 0.5-10.0μg/mL,and the correlation coefficients(r)were greater than 0.998,the limits of detection were 0.23-4.59 mg/kg.The average recoveries of the samples at three addition levels(25,50,100 mg/kg)were 78.1%-114.4%,and the relative standard deviations were 0.7%-6.6%.The raw fermented bamboo shoots samples taken from several prepacked Liuzhou river snails rice noodle manufacturers were tested with the method,and the amino acids content were 0-625.8 mg/kg.Conclusion The method is simple,rapid and efficient.It can be used for the analysis and determination of various amino acids in fermented bamboo shoots.