高效液相色谱-三重四极杆质谱法测定猪肉及肝脏中肾上腺素代谢物

Determination of metabolites of adrenaline in pork and liver by high performance liquid chromatography-triple quadrupole tandem mass spectrometry

中文关键词:  猪肉  肝脏  4-羟基-3-甲氧基扁桃酸  3,4-二羟基扁桃酸  高效液相色谱-三重四极杆质谱法

英文关键词:pork  liver  4-hydroxy-3-methoxymandelic acid  3,4-dihydroxymandelic acid  high performance liquid chromatography-triple quadrupole tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-三重四极杆质谱法同时测定猪肉及肝脏中2种肾上腺素代谢物4-羟基-3-甲氧基扁桃酸和3,4-二羟基扁桃酸。方法 待测样品经含0.2%甲酸的乙腈-水混合溶液(80:20, V:V)提取、固相萃取柱净化, 经ZORBAX SB-Aq色谱柱, 用高效液相色谱-三重四极杆质谱仪进行测定。采用内标曲线法对目标化合物进行定量分析。结果 本方法在线性范围2.5~120.0 ng/mL内, 线性良好, 相关系数为0.9999。方法检出限为0.3 μg/kg, 在低、中、高3个浓度下, 样品加标回收率范围为60.2%~104.9%, 相对标准偏差为1.3%~12.6%。结论 本方法前处理简便, 线性、回收率、灵敏度及重复性均满足方法学要求, 可同时对猪肉及肝脏中的2种肾上腺素代谢物进行测定。

英文摘要:

      Objective To establish a method for simultaneous determination of 2 adrenaline metabolites, 4-hydroxy-3-methoxymandelic acid and 3,4-dihydroxymandelic acid, in pork and liver by high performance liquid chromatography-triple quadrupole tandem mass spectrometry (HPLC-MS). Methods Samples were extracted by 0.2% formic acid with acetonitrile-water (80:20, V:V), purified by solid phase extraction cartridges, separated by a ZORBAX SB-Aq column, and then detected by HPLC-MS. Internal standard curves were used for quantitative analysis. Results In the linear range of 2.5?120.0 ng/mL, the linear coefficient was 0.9999. The limit of detection was 0.3 μg/kg, and the recovery rates were 60.2%?104.9%, with relative standard deviation 1.3%?12.6%. Conclusion This method is simple, and the linear range, recovery, sensitivity and repeatability can meet the requirement of methodology. This method can be used for the simultaneous determination of 2 adrenaline metabolites in pork and liver.