色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2009年
6期
769-775
,共7页
朱颖%陈璇%郑飞浪%白小红
硃穎%陳璇%鄭飛浪%白小紅
주영%진선%정비랑%백소홍
三相中空纤维液相微萃取%羟基苯甲酸%富集因子%聚偏氟乙烯中空纤维%电荷转移化合物
三相中空纖維液相微萃取%羥基苯甲痠%富集因子%聚偏氟乙烯中空纖維%電荷轉移化閤物
삼상중공섬유액상미췌취%간기분갑산%부집인자%취편불을희중공섬유%전하전이화합물
three-phase hollow fiber liquid-phase microextraction%hydroxybenzoic acids%enrichment factor%polyvinylidene difluoride hollow fiber%chrarge transfer compound
在优化的三相中空纤维液相微萃取(3p-HFLPME)条件下,研究了6种羟基苯甲酸类化合物(HBAs)的3p-HFLPME行为;揭示了HBAs的富集因子(EF)与其正庚醇/水条件分配系数(log P_(n-heptanol/5 mmol/L HCl))、pK_a和羟基数目(N)的相关性,初步阐明了聚偏氟乙烯中空纤维对HBAs的电荷转移传递机理以及有机溶剂对HBAs的选择性萃取机理.优化的3p-HFLPME条件:以MOF 503聚偏氟乙烯中空纤维为有机溶剂支持体,正庚醇为有机相,5 mmol/L HCl体系为给体,80 mmol/L NH_3·H_2O为接受相,搅拌速度为 1 200 r/min,萃取35 min.该方法的精密度(以相对标准偏差计)小于3%,检出限为0.09~30.00 μg/L,加标回收率为93.3% ~107.1%,HBAs质量浓度为5 mg/L 时的富集因子最高达107.6倍.
在優化的三相中空纖維液相微萃取(3p-HFLPME)條件下,研究瞭6種羥基苯甲痠類化閤物(HBAs)的3p-HFLPME行為;揭示瞭HBAs的富集因子(EF)與其正庚醇/水條件分配繫數(log P_(n-heptanol/5 mmol/L HCl))、pK_a和羥基數目(N)的相關性,初步闡明瞭聚偏氟乙烯中空纖維對HBAs的電荷轉移傳遞機理以及有機溶劑對HBAs的選擇性萃取機理.優化的3p-HFLPME條件:以MOF 503聚偏氟乙烯中空纖維為有機溶劑支持體,正庚醇為有機相,5 mmol/L HCl體繫為給體,80 mmol/L NH_3·H_2O為接受相,攪拌速度為 1 200 r/min,萃取35 min.該方法的精密度(以相對標準偏差計)小于3%,檢齣限為0.09~30.00 μg/L,加標迴收率為93.3% ~107.1%,HBAs質量濃度為5 mg/L 時的富集因子最高達107.6倍.
재우화적삼상중공섬유액상미췌취(3p-HFLPME)조건하,연구료6충간기분갑산류화합물(HBAs)적3p-HFLPME행위;게시료HBAs적부집인자(EF)여기정경순/수조건분배계수(log P_(n-heptanol/5 mmol/L HCl))、pK_a화간기수목(N)적상관성,초보천명료취편불을희중공섬유대HBAs적전하전이전체궤리이급유궤용제대HBAs적선택성췌취궤리.우화적3p-HFLPME조건:이MOF 503취편불을희중공섬유위유궤용제지지체,정경순위유궤상,5 mmol/L HCl체계위급체,80 mmol/L NH_3·H_2O위접수상,교반속도위 1 200 r/min,췌취35 min.해방법적정밀도(이상대표준편차계)소우3%,검출한위0.09~30.00 μg/L,가표회수솔위93.3% ~107.1%,HBAs질량농도위5 mg/L 시적부집인자최고체107.6배.
Under the optimal experimental conditions of three-phase hollow fiber liquid-phase microextraction (3p-HFLPME) , the behaviors of hydroxybenzoic acids (HBAs) were investiga-ted. The correlativities between the enrichment factor (EF) of HBAs and their n-heptanol/wa-ter conditional distribution coefficients (log P_(n-heptanol/5mmol/L HCl), pK_a and the number of -OH (N); the extraction mechanism that polyvinylidene difluoride hollow fiber contributed to pro-mote the extraction efficiency by forming charge transfer compound with HBAs and the organic solvents showed notable selectivity for HBAs were elucidated. The optimal 3p-HFLPME condi-tions were: MOF 503 polyvinylidene difluoride hollow fiber as organic solvent supporter, n-hep-tanol as organic phase, 5 mmol/L HCl in the donor phase and 80 mmol/L NH_3·H_2O as the ac-ceptor phase, the HBAs were extracted for 35 min under an agitation of 1 200 r/min. It was found that the relative standard deviations were lower than 3%, the detection limits were 0. 09 -30. 00 μg/L, the average recoveries of HBAs in Calyx Kaki were 93. 3%-107. 1% and the EF of HBAs at 5 mg/L was up to 107. 6 fold.