气相色谱法同时测定食品中3种抗氧化剂

SIMULTANEOUS DETERMINATION OF BHA,BHT AND TBHQ IN FOODS BY GAS CHROMATOGRAPHY WITH FID

目的：建立气相色谱-氢火焰离子化检测器法同时测定食品中3种抗氧化剂丁基羟基茴香醚（BHA）、二丁基羟基甲苯（BHT）和特丁基对苯二酚（TBHQ）的方法,用于各种食品样品中BHA、BHT和TBHQ的含量测定.方法：取一定量油类样品,用10ml甲醇分3次振摇萃取,用滤纸过滤后取1 μl进行色谱分析;色谱条件为：色谱柱SPB-1柱（15 m×0.53 mm×0.50μm）,初始温度120℃,保持5 min后,以40℃/min的速率升至220℃,保持1 min;载气氮气流速为25 ml/min,柱头压4psi,进样量1.0μl,分流比为25：1.结果：BHA在2.0～100.0μg/L浓度范围内线性良好,相关系数r=0.99995;BHT在2.0～100.0μg/L浓度范围内相关系数r=0.9997;TBHQ在2.0～100.0 μg/L浓度范围内相关系数r=0.9998.BHA、BHT和TBHQ的平均回收率基本在95%以上.用本法调查了1 859种食品中BHA、BHT和TBHQ的含量.结论：方法快速、灵敏、准确,样品处理简便易行,可用于各种食品及油脂类中BHA、BHT和TBHQ的同时测定.

Objective： To develope method for the determination of the eoncentrations of BHA, BHT and TBHQ in foods by using gas chromatography- flame ionization detector （GC- FID）. Methods： BHA, BHT and TBHQ were extracted from food sampies by methanol for 3 times, and total extracting volume is 10 ml. The methanol layer was filtrated by filter paper, and analyzed by GC. The GC system eonsisted of Supleco SPB- 1 eohtrnn （15 m × 0.53 mm× 0.50μm）, carrier of nitrogen, split ratio （25：1）, injection volume 1μl, initial column temperature 120 ℃, keeping 5 minutes and rising to 220 ℃ with rate of 40 ℃ per minute. Results. The linear ranges of determination for BHA, BHT and TBHQ were 2.0- 100.0 μg/L （ r = 0.99995）, 2.0- 100.0 μg/L （ r = 0.9997） and 2.0- 100.0μg/L （ r = 0.9998）, respectively. The recoveries of spiked samples for these anti - oxidizing agents were above 95%. 1 859 food samples were collected, and BHA, BHT, TBHQ eontents were determined by this method. Conclusion： The method is sensitive, simple, rapid and accurate, it can be used to simultaneously determine anti - oxidizing agent in foods.