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| 高效液相色谱-串联质谱法测定猪肉中氨基酸含量 |
| LI yanming1, WANG kun2,*, LI min1, WANG xiaoli1, CAO juan3 |
| 投稿时间：2024-09-04 修订日期：2025-04-09 |
| DOI： |
| 中文关键词: 猪肉 氨基酸 高效液相色谱-串联质谱法 |
| 英文关键词:pork amino acid high performance liquid chromatography-tandem mass spectrometry |
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| 中文摘要: |
| 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，r2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。 |
| 英文摘要: |
| Objective To establish a method for the simultaneous detection of multiple amino acids in each part of year-end 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 has 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. |
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