CAJ | 학술논문

建立用液相微萃取-高效液相色谱法测定乳制品中的三聚氰胺的检测方法.样品预处理采用聚丙烯中空纤维进行液相微萃取,考察有机萃取溶剂、给出相和接收相pH值、搅拌速度、盐效应和萃取时间的影响,确定以磷酸三丁酯(tributyl phosphate,TBP)为有机萃取溶剂,0.02mol/L硫酸铵溶液为接受相,给出相和接收相pH值分别为8.0和5.0,搅拌速率1000r/min,萃取时间30min的三聚氰胺优化萃取条件.选用Agilent C_(18)(4.6mm×250mm,5μm)色谱柱,在优化的色谱条件下对样品进行检测.方泫线性范围为0.01～100μg/mL,相关系数R~2=0.9987;检测限为2.5ng/mL(R_(SN)=3);相对标准偏差小于4.4%(n=5);回收率为92.1%～102.4%.本法有机溶剂消耗少,单个样品的分析时间小于34min,且具有灵敏、高效、可靠等优点,可用于乳制品类复杂基质中低含量三聚氰胺的快速测定.
건립용액상미췌취-고효액상색보법측정유제품중적삼취청알적검측방법.양품예처리채용취병희중공섬유진행액상미췌취,고찰유궤췌취용제、급출상화접수상pH치、교반속도、염효응화췌취시간적영향,학정이린산삼정지(tributyl phosphate,TBP)위유궤췌취용제,0.02mol/L류산안용액위접수상,급출상화접수상pH치분별위8.0화5.0,교반속솔1000r/min,췌취시간30min적삼취청알우화췌취조건.선용Agilent C_(18)(4.6mm×250mm,5μm)색보주,재우화적색보조건하대양품진행검측.방현선성범위위0.01～100μg/mL,상관계수R~2=0.9987;검측한위2.5ng/mL(R_(SN)=3);상대표준편차소우4.4%(n=5);회수솔위92.1%～102.4%.본법유궤용제소모소,단개양품적분석시간소우34min,차구유령민、고효、가고등우점,가용우유제품류복잡기질중저함량삼취청알적쾌속측정.
A method using liquid-phase microextraction coupled to high performance liquid chromatography (LPME-HPLC) was proposed for the determination of melamine in dairy products.LPME was achieved with polypropylene hollow fiber for 30 min at 1000 r/min string rate using tributyl phosphate (TBP) as extraction solvent and 0.02 mol/L ammonium sulfate solution at pH 5.0 (pH 8.0 of donor phase) as acceptor phase.An Agilent C_(18) (4.6 mm×250 mm,5 μm) column was used for chromatographic separation and the analyte was detected under optimized conditions.The proposed method provided a linear range of 0.01-100 μg/mL with R~2=0.9987,detection limit of 2.5 ng/mL (R_(SN)=3),RSD<4.4% (n=5) and spike recovery ranging 92.1%-102.4%.Less than 34 min is needed for single sample analysis with little organic solvent consumption.Moreover,this method has the advantages of high sensitivity and extraction efficient and good reliability,thereby benefiting the rapid determination of low content of melamine in complex dairy product matrices.