建立了微波水解技术和液相色谱-串联质谱技术测定畜禽肉和鸡蛋中17种氨基酸含量的方法。以传统酸水解技术为对照,比较分析微波水解和高压水解技术的不同。以0.1%(体积分数)甲酸水溶液+10 mmol/L乙酸铵溶液和甲醇为流动相,梯度洗脱,串联质谱正离子模式进行监测,外标法定量。结果表明,与传统的氨基酸分析仪相比,微波水解-液相色谱-串联质谱技术法无需进行样品的衍生可直接测定,缩短了样品的检测时间。该检测方法的线性范围为5~375 μg/L,相关系数R2≥0.993,检出限为0.025~0.250 μg/kg,加标回收率为85%～96%,精密度为0.01%～0.71%。该方法缩短了蛋白质的水解时间,快速简便、灵敏度较高、数据准确可靠,可用于畜禽肉和鸡蛋中17种氨基酸的测定。
A method for the determination of 17 amino acids in meat and eggs was established by microwave hydrolysis and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Compared with the traditional acid hydrolysis technology, the differences between microwave hydrolysis and high-pressure hydrolysis technology were compared and analyzed. Based on the comparative analysis of traditional acid hydrolysis, microwave hydrolysis, and high-pressure hydrolysis methods, gradient elution was carried out with 0.1% formic acid aqueous solution + 10 mmol/L ammonium acetate solution and methanol as mobile phases. Tandem mass spectrometry was used for monitoring and analysis in positive ion mode and external standard method was used for quantification. Results showed that compared with the traditional amino acid analyzer, the microwave hydrolysis-LC-MS/MS method could be used for direct determination of samples without derivatization, which shortened the detection time of samples. The linear range of this method was 5-375 μg/L, the correlation coefficients were more than 0.993, the detection limit was 0.025-0.250 μg/kg, the recovery rate of standard addition was 85%-96%, and the relative standard deviations were 0.01%-0.71%. The method shortens the protein hydrolysis time, has high sensitivity, accurate, and reliable data, and can be used for the determination of 17 amino acids in meat and eggs.
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