摘要
制备了纳米二氧化锰(nMnO2),并用傅里叶变换红外光谱(FTIR)和扫描电镜(SEM)进行了表征。将所制得的nMnO2作为吸附剂用于固相萃取(SPE)分离富集油炸食品中丙烯酰胺(AA),并用高效液相色谱法(HPLC)测定其含量。称取粉状样品2.0000g,用甲醇振荡提取3次(第一次用8mL,第二和第三次各用6mL),每次20min。离心分层,收集并合并3次所得上清液,在40℃吹氮浓缩至6mL,于4℃冷藏2h后离心,取上清液,加入正己烷,混匀,重复萃取4次,每次加正己烷6 mL。取4次所得上清液合并,并于40℃吹氮浓缩至约1.6 mL。将样品溶液以2.0mL·min-1的速率流经装填有200 mg nMnO2的SPE小柱,然后用甲醇-水(40+60)溶液0.5mL以流量6.0mL·min-1淋洗小柱以去除杂质。接着用乙腈-冰乙酸(99+1)溶液0.8mL,以流量1.0mL·min-1淋洗SPE小柱,将其所吸附的AA洗脱。洗脱液经0.25μm滤膜过滤,取滤液10μL进行HPLC分析。应用上述条件,分析物的富集倍数达148。AA的质量浓度在0.5~250μg·L-1内与其峰面积呈线性关系,其检出限(3S/N)为0.054μg·L-1。应用此方法分析了5种油炸食品样品,并在这5种样品的基质上加入AA标准溶液进行回收试验,测得回收率在80.0%~96.0%之间,测定值的相对标准偏差(n=5)在2.4%~8.8%之间。
Nano-manganese dioxide(nMnO2)was prepared and the product obtained was characterized by FTIR and SEM.nMnO2 was used as adsorbent in SPE for separation and enrichment of acrylamide(AA)in fried food and determined by HPLC.A portion(2.000 0g)of the powdered sample was taken and extracted by vibration thrice with methanol(8 mL,6 mL and 6 mL)for 20 min in each extraction.After phase-separation by centrifugation,the 3supernatants were collected,combined and evaporated at 40℃to ca.6 mL by N2-blowing.The concentrate was refrigerated at 4℃for 2h,and then centrifuged.The sepernatant was taken and extracted4times with n-hexane(6 mL were added in each extraction).The 4supernatants were collected,combined and concentrated at 40℃to ca.1.6 mL by N2-blowing.The sample solution was then passed through the SPE micro column which was packed with 200 mg of nMnO2.Flow-rate taken for the sample solution was 2.0 mL·min-1.The micro column was rinsed with 0.5 mL of a mixture of CH3OH and water(40+60)flowing at a rate of6.0mL·min-1 to eliminate impurites.The 0.8mL of a mixture of acetonitrile and glacial acetic acid(99+1)was passed through the micro column at a flow rate of 1.0 mL·min-1,to elute adsorted AA from the column.The eluate obtained was filtered through 0.25μm filtering membrane,and an aliquot of 10μl was introduced into the instrument for HPLC analysis.Enrichment factor obtained by this method was attained to a value of 148.Linear relationship was obtained between values of peak areas and mass concentration of AA in the range of 0.5to 250μg·L-1,with detection limit(3S/N)of 0.054μg·L-1.Samples of 5different fried food were analyzed by the proposed method,and test for recovery was made by addition of AA standard solution to the 5samples as matrixes,giving results of recovery in the range of 80.0%to 96.0%.Values of RSDs(n=5)found were in the range of 2.4%to8.8%.
作者
刘海霞
狄婧
饶红红
郑艳萍
姜永强
赵国虎
LIU Haixia;DI Jing;RAO Honghong;ZHENG Yanping;JIANG Yongqiang;ZHAO Guohu(School of Chemistry and Chemical Engineering,Lanzhou City University,Lanzhou 730070,China;Provincical Key Laboratory of Gansu Higher Education for City Environmental Pollution Control,Lanzhou 730070,China;School of Chemical and Biological Engineering,Lanzhou Jiaotong University,Lanzhou 730070,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2019年第12期1373-1378,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家自然科学基金项目(21765013)
甘肃省自然科学基金项目(18JR3RA220)
