提出了固相萃取-高效液相色谱法测定炒货食品中丁基羟基茴香醚(BHA)、二丁基羟基甲苯(BHT)、叔丁基对苯二酚(TBHQ)和没食子酸丙酯(PG)等人工合成的抗氧化剂和茶多酚、甘草抗氧化物、迷迭香提取物等天然抗氧化剂的方法.样品经甲醇-异丙醇-乙腈(2+1+2)混合溶剂提取后经C18固相萃取柱富集,用甲醇从柱上洗脱抗氧化剂使其净化.洗脱液在50 ℃氮气吹干,定容至1.0 mL,取10 μL试样溶液注入高效液相色谱仪测定.采用反相C18色谱柱为分离柱,以乙腈和三氟乙酸-水(0.05+99.95)溶液为流动相作梯度淋洗,在280 nm作紫外检测(甘草酸在250 nm检测).各抗氧化剂的质量浓度分别在一定的范围内呈线性关系,方法的测定下限(10S/N)在0.1~1.0 mg·kg-1之间.以油炸花生空白试样为基体,加入标准溶液进行回收试验,测得试样中抗氧化剂的回收率在83.6%~106.0%之间,相对标准偏差(n=6)在1.3%~3.9%之间.

A method of HPLC for determination of synthetic and natural antioxidants,i.e.BHA,BHT,TBHQ,PG,tea polyphenol,licorice root antioxidant,rosemary extract and etc.,in roasted seeds and nuts was proposed.The samples were extracted with a mixture of methanol-isopropanol-acetonitrile (2+1+2),and antioxidants in the extract were separated and enriched by solid phase extraction (SPE) on C18 column.The SPE column was eluted with methanol,and the eluate obtained was evaporated to dryness by N2-blowing at 50 ℃ and made up to 1.0 mL.An aliquot of 1.0 μL was used for HPLC determination.C18 reversed-phase column was used as the stationary phase and mixtures of acetonitrile and trifluoroacetic acid-water solution (0.05+99.95) in different ratios were used as the mobile phase in gradient elution.UV detection at 250 nm for glycyrrhizic acid and 280 nm for the other antioxidants was adopted.Linear relationships of antioxidants were found in definite ranges,with values of limit of determination (10S/N) in the range of 0.1 to 1.0 mg·kg-1.On the base of blank samples of fried peanut,tests for recovery were made by standard addition method.Values of recovery and RSD′s (n=6) found were in the range of 83.6%-106.0% and 1.3%-3.9% respectively.