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气相色谱质谱法测定酱油中3-氯-1,2-丙二醇
Determination of 3-Chloro-1,2-Propanediol in Soy Sauce by Gas Chromatography Mass Spectrometry
【摘要】 目的:建立气相色谱-质谱联用法测定酱油中3-氯-1,2-丙二醇(3-Chloro-1,2-Propanediol,3-MCPD)的方法。方法:采用ExtrelutTM20柱为固相萃取柱,40 mL乙酸乙酯为洗脱溶剂进行试样净化和衍生化,通过DB-5MS石英毛细管柱分离,全扫描模式检测。结果:3-MCPD在0~200 ng·mL-1线性关系良好,检出限为0.248μg·L-1,加标回收率为103%~113%,日内相对标准偏差为1.9%~4.9%,日间相对标准偏差为2.2%~6.2%。结论:本方法在测定酱油中3-MCPD时,具有时效性和安全性高、灵敏度高、结果准确可靠等优点,适用于实验室环境中对酱油中3-MCPD含量的监测。
【Abstract】 Objective:To establish a gas chromatography-mass spectrometry method for the determination of3-chloro-1,2-propanediol (3-MCPD) in soy sauce.Method:The ExtrelutTM20 column was used as the solid phase extraction column,and 40 mL of ethyl acetate was used as the elution solvent for sample purification and derivatization.The samples were separated using a DB-5MS quartz capillary column and detected in full scan mode.Result:3-MCPD showed a good linear relationship from 0 ng·mL-1 to 200 ng·mL-1,the detection limit is 0.248μg·L-1,the spiked recovery rate is 103%to113%,the intra day relative standard deviation is 1.9%to 4.9%,and the inter day relative standard deviation is 2.2%to 6.2%.Conclusion:This method has the advantages of high timeliness and safety,high sensitivity,accurate and reliable results in the determination of 3-MCPD in soy sauce,and is suitable for monitoring the content of 3-MCPD in soy sauce in laboratory environments.
【Key words】 soy sauce; 3-chloro-1,2-propanediol(3-MCPD); gas chromatography-mass spectrometry; ethyl acetate; improved pretreatment;
- 【文献出处】 现代食品 ,Modern Food , 编辑部邮箱 ,2024年23期
- 【分类号】TS264.21;O657.63
- 【下载频次】4