烟台大学学报（自然科学与工程版）2017，Vol.30Issue(2)：93-98,6.DOI:10.13951/j.cnki.37-1213/n.2017.02.003
异丙醇-NaCl-H2O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-H2O Aqueous Two-phase Method for Samples Pretreatment Combinedwith Gas Chromatography/Mass Spectrometry
摘要
Abstract
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-NaCl-H2O system is significantly lower than that of solvent extraction procedure.Therefore, the purification steps are greatly simplified.The C18 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 are 85.7%-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Key words
antioxidants/aqueous two-phase system/biscuits/gas chromatograph coupled with mass spectrometry(GC-MS)分类
化学化工引用本文复制引用
王雪梅,潘琳,李玲,宋跃进,刘永明,李桂芝..异丙醇-NaCl-H2O双水相体系样品前处理结合GC/MS测定饼干中的抗氧化剂[J].烟台大学学报（自然科学与工程版）,2017,30(2):93-98,6.基金项目
山东省科技惠民计划项目(2014kjhmzc02) （2014kjhmzc02）
国家自然科学基金资助项目(51472212). （51472212）
