超高效液相色谱-串联质谱法测定食用肉制品中游离谷氨酸及其盐
李颜岩,于浩洋,谢韬
辽宁省疾病预防控制中心,沈阳 110005
Determination of free glutamic acid and glutamates in edible meat products by ultra high performance liquid chromatography-tandem mass spectrometry
李颜岩,于浩洋,谢韬
Liaoning Center for Disease Control and Prevention, Shenyang 110005, China
摘要:建立超高效液相色谱-串联质谱(UPLC-MS/MS)法测定食用肉制品中游离谷氨酸及其盐的方法。将肉制品样品绞碎,混匀,称重后用水萃取样品中的游离谷氨酸及其盐,水相经涡旋、超声、离心、净化、过滤,在正离子电离模式(ESI+)和质谱多反应监测(MRM)模式下用UPLC-MS/MS法测定,外标法定量。流动相:A为0.2%甲酸水溶液,B为0.2%甲酸的乙腈,流量为0.35 mL/min,梯度洗脱。色谱柱:ACQUITY UPLC HSS T3(100 mm×3.0 mm,1.8 μm),柱温:40℃;进样体积:5.0μL。谷氨酸钠的质量浓度在0.01~1.00 mg/L范围内与色谱峰面积线性关系良好,线性相关系数为0.999 5,检出限为4.4 mg/kg(以谷氨酸计),测定结果的相对标准偏差为1.2%~2.2%,加标回收率为95.6%~98.0%。该方法易于操作,灵敏度高,选择性强,适用于肉制品中游离谷氨酸及其盐的检测。
Abstract:A method for the determination of free glutamic acid and glutamates in edible meat products by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was establish. The meat product sample was minced and mixed. After weighing, the free glutamic acid and glutamates were extracted with water and subjected to vortex, ultrasound, centrifugation, purification and filtration. Under the positive ion ionization mode (ESI+) and mass spectrometry multi-reaction monitoring (MRM), the ectract was determined by UPLC -MS/MS with the external standard method 0.2% formic acid water as A mobile phase and 0.2%formic acid acetonitrile as B mobile phase were used for gradient elution, the flow rate was 0.35 mL/min. The chromatographic column was ACQUITY UPLC HSS T3 (100 mm×3.0 mm, 1.8 μm), the temperature of oven was 40℃and the injection volume was 5.0 μL. The mass concentration of glutamic and chromatographic peak area had good linear relationship in the range of 0.01-1.00 mg/L with the linearly dependent coefficient r=0.999 5, the detection limit was 4.4 mg/kg (expressed as glutamic acid). The recovery of standard addition was 95.6%-98.0% with the relative standard deviation of detemination results precision 1.2%-2.2%. This method is simple, easy to operate, with high selectivity and sensitivity. It is suitable for the determination of free glutamic acid and glutamates in meat products.
关键词:谷氨酸及其盐;肉制品;超高效液相色谱-串联质谱法
Keywords:glutamic acid and glutamates; meat products; UPLC-MS
基金:辽宁省卫生行业基金,食品中谷氨酸及其盐专项检测及评估研究(2018205003)
本文引用格式:
李颜岩,于浩洋,谢韬.超高效液相色谱-串联质谱法测定食用肉制品中游离谷氨酸及其盐[J].化学分析计量,2019,28(6):31-34.
LI Y Y,YU H Y,XIE T. Determination of free glutamic acid and glutamates in edible meat products by ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chemical analysis and meterage,2019,28(6):31-34.
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