食品研究与开发
食品研究與開髮
식품연구여개발
FOOD RESEARCH AND CEVELOPMENT
2014年
12期
49-53
,共5页
刘燕伟%周真巡%赵文峰%马彤梅
劉燕偉%週真巡%趙文峰%馬彤梅
류연위%주진순%조문봉%마동매
超声萃取%高效液相%邻苯二甲酸二(2-乙基)己基酯%饮料
超聲萃取%高效液相%鄰苯二甲痠二(2-乙基)己基酯%飲料
초성췌취%고효액상%린분이갑산이(2-을기)기기지%음료
ultrasonic extraction%HPLC%DEHP%drinks
建立了一种快速、简便的超声波辅助水浴萃取-高效液相色谱测定饮料中邻苯二甲酸二(2-乙基)己基酯(DEHP)的方法。在盐析的作用下,使用正己烷对饮料样品在40℃下进行超声提取,经过离心、浓缩、过滤,再用C18色谱柱分离,乙腈与水(体积比为95∶5)作为流动相,224 nm紫外波长下检测DEHP的含量。本实验同时对提取条件中提取液种类及体积、盐效应、超声时间、溶液pH和离心时间进行优化。结果表明:DEHP在0.05 mg/L~5 mg/L浓度范围内线性关系良好,相关系数R=0.99995;检测限为0.0005 mg/L;加标回收率为90.2%~101%;相对标准偏差(RSD)为2.32%~5.17%。该方法简便、快速、可靠、高灵敏度等特点,适用于饮料中DEHP含量的测定。
建立瞭一種快速、簡便的超聲波輔助水浴萃取-高效液相色譜測定飲料中鄰苯二甲痠二(2-乙基)己基酯(DEHP)的方法。在鹽析的作用下,使用正己烷對飲料樣品在40℃下進行超聲提取,經過離心、濃縮、過濾,再用C18色譜柱分離,乙腈與水(體積比為95∶5)作為流動相,224 nm紫外波長下檢測DEHP的含量。本實驗同時對提取條件中提取液種類及體積、鹽效應、超聲時間、溶液pH和離心時間進行優化。結果錶明:DEHP在0.05 mg/L~5 mg/L濃度範圍內線性關繫良好,相關繫數R=0.99995;檢測限為0.0005 mg/L;加標迴收率為90.2%~101%;相對標準偏差(RSD)為2.32%~5.17%。該方法簡便、快速、可靠、高靈敏度等特點,適用于飲料中DEHP含量的測定。
건립료일충쾌속、간편적초성파보조수욕췌취-고효액상색보측정음료중린분이갑산이(2-을기)기기지(DEHP)적방법。재염석적작용하,사용정기완대음료양품재40℃하진행초성제취,경과리심、농축、과려,재용C18색보주분리,을정여수(체적비위95∶5)작위류동상,224 nm자외파장하검측DEHP적함량。본실험동시대제취조건중제취액충류급체적、염효응、초성시간、용액pH화리심시간진행우화。결과표명:DEHP재0.05 mg/L~5 mg/L농도범위내선성관계량호,상관계수R=0.99995;검측한위0.0005 mg/L;가표회수솔위90.2%~101%;상대표준편차(RSD)위2.32%~5.17%。해방법간편、쾌속、가고、고령민도등특점,괄용우음료중DEHP함량적측정。
A simple and rapid method for the determination of DEHP in drinks was developed using ultrasonic assisited hot water extraction combined with HPLC. With the effect of salting , DEHP in drinks was extracted by n-hexane using ultrasonic bath under temperature of the 40℃;followed by centrifugation, concentration and filtration. The extraction parameters such as type and volume of extracting solvent, pH of solvent, salt addition, ultrasonic time and centrifugation time were optimized. C18 column was employed in the HPLC determination with acetonitrile-water (Volume ratio is 95 to 5) as eluent and a UV detector was adjusted at 224 nm. Under the optimal conditions, the results showed that there is a good linear relationship (R=0.999 95) in the concentration range of 0.05 mg/L-5 mg/L. The detection limit of DEHP is 0.000 5 mg/L. The recoveries of DEHP in drinks were in the range of 90.2%-101%;with relative standard deviation of 2.32%-5.17%. The developed method is simple, reliable and sensitive for fast determination of DEHP in drinks.