滤纸薄膜微萃取-高效液相色谱-串联质谱法测定植物油中4-硝基酚和2,4-二硝基酚的含量  

HPLC-MS/MS Determination of 4-Nitrophenol and 2,4-Dinitrophenol in Vegetable Oils with Separation by Thin Film Microextraction on Filter Paper

作　　者：周颖[1] 安莹[1] 燕传勇[1] 葛冬梅 

机构地区：[1]徐州工业职业技术学院,徐州221140 [2]徐州市产品质量监督检验中心,徐州221008

出　　处：《理化检验（化学分册）》2016年第12期1428-1431,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：取样品1．00mL与正己烷9．00mL混匀，加入1mol·L^-1氢氧化钠溶液1O弘L，于此溶液投入滤纸条，并振荡120min。取出滤纸条，用正己烷荡洗2次去油后，用乙腈-盐酸（100＋1）混合液1．00mL洗脱，分出洗出液；滤纸用甲醇1.0mL洗涤，洗液与洗出液合并后进行色谱分离。以ACQUITY UPLC BEH C18色谱柱为分离柱，以不同体积比的甲醇和0．1％（体积分数）甲酸溶液的混合液为流动相进行梯度洗脱。在质谱分析中采用电喷雾正离子源和多反应监测模式检测。4-硝基酚（4-NP）和2，4-二硝基酚（2，4-DNP）的质量浓度均在10-1000μg·L^-1内与其峰面积呈线性关系，4-NP及2，4-DNP的检出限（3s）分别为2．5，3．0μg·L^-1。加标回收率在81．3％-97．89／6之间，测定值的相对标准偏差（n=6）在1．6％-3．5％之间。The sample （1.00 mL） was mixed with 9.00 mL of n-hexane, and 10μL of 1 mol·L^-1 NaOH solution were added. A strip of filter paper was added to the solution and the mixture was shaked for 120 min. The filter paper strip was taken out; after washing twice with n-hexane to remove oil, the filter paper was shaked with 1.00 mL of a mixture of CH3CN and HC1 （100＋1） to elute the analytes from the paper. The eluate was reserved and filter paper was washed with 1.0 mL of methanol, which was then combined with the eluate and used as sample solution for HPLC separation. ACQUITY UPLC BEH C18 chromatographic column was used as stationary phase, and mixtures of methanol and 0. 1%（φ） formic acid solution mixed in different ratio were used as mobile phase in gradient elution. ESI＋ and multi-reactions monitor were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of 4-nitrophenol （4-NP） and 2,4-dinitrophenol （2,4-DNP） were kept in the same range of 10-1 000 μg·L^-1, with detection limits （3s） of 2. 5 μg·L^-1 （for 4-NP） and 3. 0 μg·L^-1 （for 2,4- DNP）. Values of recovery found by standard addition method were in the range of 81.3%-97. 8%, and values of RSD＇s （n=6） found were in the range of 1.6%-3. 5%.

关 键 词：高效液相色谱-串联质谱法 薄膜微萃取 植物油 4-硝基酚 2 4-二硝基酚 

分 类 号：O657.63[理学—分析化学]