凝胶渗透色谱净化-气质联用法同时测定方便面中的BHA、BHT和TBHQ

Simultaneous determination of BHA,BHT and TBHQ in instant noodles by gas chromatography-mass spectrometry with gel permeation chromatography

目的建立凝胶渗透色谱结合气相色谱-质谱同时测定方便面中抗氧化剂丁基羟基茴香醚(BHA)、2.6-二叔丁基-4甲基苯酚(BHT)和特丁基对苯二酚(TBHQ)的分析方法。方法样品采用乙醇提取,以环已烷-乙酸乙酯(1∶1,V/V)为流动相进行凝胶渗透色谱净化,经VF-1701MS毛细管柱分离,选择离子监测模式(SIM)对目标化合物进行检测和确认。结果优化了样品前处理过程和色谱分离条件,建立方便面中3种抗氧化剂的同时测定方法。该方法在1μg/ml^200μg/ml时,相关系数>0.999;方法的回收率为81.8%~92.4%,相对标准偏差为3.4%~5.9%。丁基羟基茴香醚的检出限为0.01 mg/kg,2,6-二叔丁基-4甲基苯酚的检出限为0.02 mg/kg,特丁基对苯二酚的检出限为0.15 mg/kg。结论本方法净化效果好、灵敏度高、操作简单快速、实验结果准确,适合于方便面中3种抗氧化剂的定性和定量分析。

Objective A method has been established for the rapid determination of 3 antioxidants（ TBHQ,BHA and BHT） in instant noodles. Methods The target analytes were extracted with ethanol and then purified with gel permeation chromatography（ GPC） by cyclohexane-ethyl acetate（1∶1,V / V） as mobile phase. The analytes were separated on a VF-1701 MS column and detected in selected ion monitoring mode. Results Sample pretreatment and chromatographic separation conditions were optimized to establish a method for simultaneous determination of 3 antioxidants in instant noodles. The linearity of the method were greater than 0. 999 in the range of 1μg / ml to 200 μg / ml. The detection limits of recovery rates ranged from81. 8% to 92. 4%,with detection limits of relative standard deviations（ RSDs） of 3. 4%-5. 9%. The limits of detection for BHA,BHT and TBHQ were 0. 01 mg / kg,0. 02 mg / kg and 0. 15 mg / kg,respectively. Conclusion This method exhibited high sensitivity,easy operation,high speed and accurate results. It is suitable for the determination of 3 antioxidants in instant noodles.