异丙醇-NaCl-H_2O双水相体系样品前处理结合GC/MS测定饼干中的抗氧化剂  

Determination of Antioxidants in Biscuit Samples through Isopropanol-NaCl-H_2O Aqueous Two-phase Method for Samples Pretreatment Combined with Gas Chromatography/Mass Spectrometry

作　　者：王雪梅[1] 潘琳[1] 李玲[1] 宋跃进[1] 刘永明[1] 李桂芝[1] WANG Xue-mei PAN Lin L SONG Yue-jin LIU Yong-ming LI Gui-zhi(School of Chemistry and Chemical Engineering, Yantai University, Yantai 264005 ,Chin)

机构地区：[1]烟台大学化学化工学院,山东烟台264005

出　　处：《烟台大学学报（自然科学与工程版）》2017年第2期93-98,共6页Journal of Yantai University(Natural Science and Engineering Edition)

基　　金：山东省科技惠民计划项目(2014kjhmzc02);国家自然科学基金资助项目(51472212)

摘　　要：用异丙醇-NaCl-H_2O双水相体系结合气相色谱-质谱联用(GC-MS)法高效提取并测定了饼干中的两种抗氧化剂:叔丁基羟基茴香醚(BHA)和2,6-二叔丁基羟基甲苯(BHT).实验考察了双水相体系的形成条件,并探讨了双水相体系对BHA、BHT的萃取效率.结果表明:异丙醇对样品中BHA、BHT有较高的提取效率,NaCl具有较好的盐析分相作用.饼干中的抗氧化剂(BHA、BHT)的萃取率与异丙醇水溶液的体积分数有关,当双水相体系中水与异丙醇的体积之比约为3∶2时,异丙醇与饼干中的抗氧化剂(BHA、BHT)可充分接触,萃取率较高.比较了双水相萃取法与非水溶性溶剂提取法的提取液中脂溶性杂质的含量,结果表明,双水相体系萃取液中脂溶性杂质含量较低,加入C_(18)与PSA吸附剂即可去除杂质,简化了净化步骤.该方法适用于测定饼干中的抗氧化剂(BHA、BHT),回收率为85.7%~99.7%,检出限为2.6~5.3ng/g.On the basis of isopropanol-NaCl-H2O aqueous two-phase system,the antioxidants including BHA（ butylated hydroxyanisole） and BHT（ butylated hydroxytoluene） in biscuit samples are quickly determined by gas chromatograph（ GC） coupled with mass spectrometry（ MS）. The influence factors of the aqueous two-phase system on extraction of BHA and BHT in biscuit samples are investigated in detail. The results show that isopropanol has superior ability for extraction of BHA and BHT in biscuit samples. Sodium chloride can get high efficiency for salting out phase separation. In the procedures of biscuit samples pretreatment,the extraction rate of BHA and BHT is related to the volume fraction of isopropyl alcohol. When the volume ratio of water and isopropyl alcohol is approximately 3∶ 2,the isopropyl alcohol and antioxidants in biscuits can fully contact,and the extraction rate is rather high. Meanwhile,the amounts of liposoluble impurity in the extract of aqueous two-phase system and solvent extraction procedure are compared,and it is shown that the content of liposoluble impurity in the extract of isopropanol-Na Cl-H2O system is significantly lower than that of solvent extraction procedure. Therefore,the purification steps are greatly simplified. The C（18） modified silica and primary secondary amine（ PSA） are added in upper phase to eliminate the impurities,then the antioxidants in extract（ upper phase） are directly analyzed by GC/MS. This method has been applied to the determination of BHA and BHT in biscuit samples,the spiked recoveries are85. 7%-99. 7%,and the detection limits are in the range of 2. 6-5. 3 ng/g.

关 键 词：抗氧化剂 双水相体系 饼干 气相色谱-质谱联用 

分 类 号：O621.4[理学—有机化学]