气相色谱-离子阱串联质谱法测定酱油中的曲酸  

Determination of kojic acid in soy sauces by gas chromatography-ion trap tandem mass spectrometry

作　　者：陈柯星[1,2] 郑申西[1] 柯华[1] 林捷[1] 张兰[2] 

机构地区：[1]福州市疾病预防控制中心,福建福州350004 [2]福州大学化学化工学院,福建福州350108

出　　处：《中国卫生检验杂志》2015年第16期2686-2688,2692,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立酱油中曲酸的气相色谱-离子阱串联质谱(GC-MS/MS)测定方法。方法酱油样品用氯化钾-盐酸缓冲溶液稀释,并用盐酸溶液调p H≈2.0后,真空冷冻干燥,冻干残渣用甲醇和乙酸乙酯溶解、离心,移取上清液经氮气吹干,加入衍生化试剂衍生后,采用气相色谱-离子阱串联质谱仪,运用多级质谱扫描模式(MSn)进行扫描测定,外标法定量。结果本研究方法条件下,曲酸在5 mg/L^100 mg/L时具有良好的线性,相关系数为0.999,以3倍空白基线噪音测得方法的检出限为2.0 mg/L。进行3个水平加标回收实验(20.0 mg/L、50.0 mg/L、80.0 mg/L),样品加标回收率为82.5%~88.5%,相对标准偏差(RSD)为5.25%~5.71%。结论本方法选择性高、结果准确可靠,适于基质复杂的酱油样品中微量曲酸的测定。Objective To establish a method for determination of kojic acid in soy sauces by gas chromatography- ion trap tandem mass spectrometry（ GC- MS / MS）. Methods The sample was diluted with potassium chloride- hydrochloric acid buffer solution,and be regulated to p H≈2. 0 by hydrochloric acid solution. The diluent was dried by vacuum freeze dying,then the residues were dissolved ultrasonically with methanol and ethyl acetate. After centrifugation,all the supernatant solution was removed and be dried by nitrogen. After derivatized with BSTFA,the target compound was determined by GC- MS / MS with MSn mode,and quantified by external standard method. Results In the condition of this method,the calibration curve showed good linearity in the range of 5 mg / L ~ 100 mg / L with correlation coefficient 0. 999,The detection limit of the method was 2 mg / L with 3 times the blank baseline noise. The average recovery of kojic acid was 82. 5%- 88. 5% at three spiked levels of20. 0 mg / L,50. 0 mg / L and 80. 0 mg / L,and the relative standard deviations（ RSD） was 5. 25%- 5. 71%. Conclusion The method is selective and accurate,and it is suitable for the determination of complex matrix trace kojic acid in soy sauces.

关 键 词：曲酸 硅烷化衍生 气相色谱-离子阱串联质谱 酱油 

分 类 号：O657.63[理学—分析化学]