UHILIC-MS/MS同时测定栝楼桂枝颗粒中22个氨基酸的含量

目的 建立一种超高效亲水作用色谱串联三重四极杆质谱法(UHILIC-MS/MS)对栝楼桂枝颗粒中22个氨基酸类成分(亮氨酸、苯丙氨酸、色氨酸、异亮氨酸等)进行含量测定.方法 采用超高效亲水作用色谱串联三重四极杆质谱法,正离子多反应监测(MRM)模式进行含量测定.色谱条件:采用亲水作用色谱柱,Acquity BEH(2....

Simultaneous determination of 22 amino acids in Gua Lou Gui Zhi Granules by UHILIC-MS/MS

Objective To develop an ultra hydrophilic interaction chromatography mass spectrometry(UHILIC-MS/MS)method for the determination of 22 amino acids in Gua Lou Gui Zhi Granules(GLGZG).Methods UHILIC-MS/MS method,positive ion mode,and multiple reaction monitoring(MRM)mode were used to determine the 22 contents.chromatographic method:hydrophilic interaction column(Acquity BEH column,2.1 mm×100 mm,1.7μm),column temperature set at 45℃,mobile phase consisting of 0.25%formic and 2 mmol·L^-1 ammonium formate in water(A phase)-acetonitrile(B phase)for gradient elution.Injection volume was set at 1μL and flow rate was 0.4 mL·min^-1.Results The contents of 22 amino acids were determined within 6 min in GLGZG under the optimized chromatographic conditions.They had good linearity in their linear ranges(r>0.9953).The recovery rate were 96.13~103.93%with RSD s of 1.19%~2.93%.The precision,stability,repeatability were less than 4.32%,4.94%,4.78%,4.87%,and 4.91%.The content determination results of 3 batches of samples found that among 22 amino acids,the contents of citrulline,gamma-aminobutyric acid,proline,asparagine and arginine are more than 0.3 mg·g^-1.Conclusion The quantitative analysis method of UHILIC-MS/MS was simple,rapid,accurate,and the separation effect was good,which can provide a basis for improving the quality standard of GLGZG.