气相色谱法测定广式腊肉中三种抗氧化剂的含量

Determination of three antioxidants in Cantonese bacon by gas chromatography

目的:建立气相色谱法测定广式腊肉中三种抗氧化剂含量的分析方法。方法:以丁基羟基茴香醚(BHA)、二丁基羟基甲苯(BHT)、特丁基对苯二酚(TBHQ)为标准物质,Inert Cap 5(30m×0.25mm×0.25μm)为分离柱,以初始温度70℃,保持1min,4℃/min升温至150℃,保持2min,再以10℃/min升温至250℃,保持2min为程序升温,氢火焰离子化检测器温度为250℃。腊肉经搅碎,石油醚与乙醚混合试剂多次提取,氮吹浓缩至近干,乙酸乙酯定容的条件下以外标法定量。结果:抗氧化剂的加标回收率在95.6%～108.8%之间,相对标准偏差在0.7%～0.9%之间,丁基羟基茴香醚(BHA)、二丁基羟基甲苯(BHT)、特丁基对苯二酚(TBHQ)的方法检出限分别为1.76 mg/kg、2.02 mg/kg、2.11 mg/kg。结论:该方法操作过程简单,无需净化,结果重现性好,灵密度高,回收率高,适用于广式腊肉中三种抗氧化剂含量的测定,能为广大的检测工作者提供一种检测腊肉中三种抗氧化剂的参考方法。

Objective ： to establish an analytical method for the determination of three antioxidants in Cantonese bacon by GC. Methods ：Butyl Hydroxyl Anisole （BHA）, Dibutyl Hydroxyl Toluene （BHT）, Tert-butyl hydroquinone （TBHQ） were selected as standard material, and Inert Cap 5 （30m×0.25mm× 0.251μm） was used as the separation column. Initial temperature of 70℃ was maintained for 1 rain, then at the speed of 4℃ / min increase to 150℃ and kept for 2 min, then increase the temperature to 250℃ at 10℃ / rain, keep the temperature for 2 min for programming：the temperature of the hydrogen flame ionization detector is 250℃. After grinding, the beacon was extracted by petroleum ether and diethyl ether mixture for multiple times and dried by nitrogen blowing. The external standard method of using ethyl acetate to the constant volume is applied for quantification tests. Results ： The recoveries of antioxidants were between 95.6% and 108.8%, and the relative standard deviations were between 0.7% and 0.9%. Butyl Hydroxyl Anisole （BHA）, Dibutyl Hydroxyl Toluene （BHT）, Tert-butyl hydroquinone （TBHQ） were 1.76 mg/kg, 2.02 mg/kg, and 2.11 mg/kg, respectively. Conclusion ： The method is simple in operation, no need to purify, had a good reproducibility, high density;it is accurate and rapid with a high recovery rate. The method is suitable for the determination of three antioxidant contents in Cantonese bacon.