高效液相色谱-串联质谱法测定猪肉中氨基酸含量  

Determination of amino acids content in pork by high performance liquid chromatography-tandem mass spectrometry

作　　者：李艳明 王坤 李敏 王小利 曹娟 LI Yan-Ming;WANG Kun;LI Min;WANG Xiao-Li;CAO Juan(Binzhou Inspection and Testing Center,Binzhou 256600,China;School of Health,Binzhou Polytechnic,Binzhou 256603,China;Binzhou Zhongyu Food Industry Co.,Ltd.,Binzhou 256600,China)

机构地区：[1]滨州市检验检测中心,滨州256600 [2]滨州职业学院健康学院,滨州256603 [3]滨州中裕食品有限公司,滨州256600

出　　处：《食品安全质量检测学报》2025年第9期277-288,共12页Journal of Food Safety and Quality

摘　　要：目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)同时检测猪肉各部位中多种氨基酸的方法。方法 样品以酸化高温水解、酸化微波水解、碱化高温水解方式分别进行提取,采用HPLC-MS/MS进行分析,电喷雾离子源正离子模式,多反应监测(multiple reaction monitoring,MRM)模式采集,以甲酸水溶液-甲酸的甲醇乙腈(1:4,V:V)溶液作为流动相进行梯度洗脱。结果 以酸化微波水解方式提取,时间短、效率高。该检测方法在线性范围内关系良好,相关系数r^(2)在0.9905~0.9956之间,检出限为0.012~0.133 ng/mL,定量限为0.038~0.444 ng/mL,回收率为85.58%~98.84%,相对标准偏差(relative standard deviations,RSDs)在0.68%~6.71%之间。结论 该方法过程简单,具有良好的重复性和稳定性,不仅可用于猪肉各部位中多种氨基酸的同时检测,达到高通量快速检测的目的,而且还能够有效监测猪肉产品的掺假行为。Objective To establish a method for the simultaneous detection of multiple amino acids in each part of pork by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The samples were extracted by acidizing high-temperature hydrolysis,acidizing microwave hydrolysis and alkalization high-temperature hydrolysis,determined by HPLC-MS/MS,electrospray ionization in positive ion mode,multiple reaction monitoring(MRM),used formic acid solution-methanol acetonitrile(1:4,V:V) solution of formic acid as mobile phase with gradient elution.Results It was extracted by acidizing microwave hydrolysis with short time and high efficiency.The detection method had a good relationship in the linear range,r2 was between 0.9905 and 0.9956,the limits of detection were 0.012–0.133 ng/mL,the limits of quantitation were 0.038–0.444 ng/mL,the average recoveries were in the range 85.58% and 98.84%,the relative standard deviations(RSDs) were 0.68%–6.71%.Conclusion The method has simple process,good repeatability and stability,and can not only be used for simultaneous detection of multiple amino acids in each part of pork to achieve the purpose of high-throughput and rapid detection,but also can effectively monitor the adulteration behavior of pork products.

关 键 词：猪肉 氨基酸 高效液相色谱-串联质谱法 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程]