高效液相色谱-荧光检测器-二级阵列管检测器法测定烤羊肉串中16种多环芳烃  

Determination of 16 polycyclic aromatic hydrocarbons in kebabs by high performance liquid chromatography-fluorescence detector-secondary array tube detector

作　　者：张永胜 韩金花 田铸 张丹[2] 张珍[1] 师希雄[1] ZHANG Yongsheng;HAN Jinhua;TIAN Zhu;ZHANG Dan;ZHANG Zhen;SHI Xixiong(Food Science and Engineering College,Gansu Agricultural University,Lanzhou 730070,China;Gansu Provincial Key Lab of Aridland Crop Science,Gansu Agricultural University,Lanzhou 730070,China)

机构地区：[1]甘肃农业大学食品科学与工程学院,甘肃兰州730070 [2]甘肃省干旱生境作物学重点实验室(甘肃农业大学),甘肃兰州730070

出　　处：《食品与发酵工业》2022年第23期274-280,共7页Food and Fermentation Industries

基　　金：甘肃传统绿色肉制品绿色制造技术研究及产业化示范项目(20YF3NA014)。

摘　　要：通过优化前处理条件(超声波时间、固相萃取柱、洗脱剂种类和洗脱剂体积),建立烤羊肉串中16种多环芳烃(polycyclic aromatic hydrocarbons,PAHs)残留的高效液相色谱-荧光检测器-二级阵列管检测器检测方法。以乙腈和乙腈饱和正己烷为提取液,样品经30 min超声波辅助提取,及多环芳烃分子印迹柱(polycyclic aromatic hydrocarbons molecularly imprinted column,PAH-MIP)固相萃取,用9 mL V(正己烷)∶V(二氯甲烷)=30∶70洗脱;苊烯用二极管阵列检测器测定,其他15种PAHs用荧光检测器测定,色谱柱为Agilent SB C18柱,进样量为5μL,柱温30℃,流速0.8 mL/min,流动相选用乙腈和水,洗脱模式为梯度洗脱。在1~50 ng/mL范围内,16种PAHs线性关系良好,相关系数均大于0.99,在2、5、20 ng/mL 3个加标水平下,平均回收率为81%~104%,相对标准偏差为0.95%~5.84%,方法检出限(S/N=3)为0.33~3.30μg/kg,定量限(S/N=10)为1.0~10.0μg/kg。高效液相色谱-荧光检测器-二级阵列管检测法适用于羊肉串中PAHs的分析。By optimizing the pretreatment conditions(sonication time,solid phase extraction column,eluent type and eluent volume),a high-performance liquid chromatography-fluorescence detector-secondary array tube detector method for the detection of 16 polycyclic aromatic hydrocarbons(PAHs)residues in kebabs was established.acetonitrile and acetonitrile-saturated N-hexane were used as extracts,and the samples were extracted by ultrasound for 30 min,solid phase extraction via polycyclic aromatic hydrocarbons molecular imprinted column(PAH-MIP),elute with 9 mL of n-hexane-dichloromethane(30:70,v/v),the acenaphthene was measured by a diode array detector,and the other 15 PAHs were measured by a fluorescence detector,the chromatographic column was an Agilent SB C18 column,the injection volume was 5μL,the column temperature was 30℃,and the flow rate was 0.8 mL/min.,acetonitrile and water were used as mobile phases,and the elution mode was gradient elution.in the range of 1-50 ng/mL,the 16 PAHs had a good linear relationship,and the correlation coefficients were all greater than 0.99.At three spiking levels of 2,5 and 20 ng/mL,the average recoveries were 81%-104%,the relative standard deviations were 0.95%-5.84%,and the method detection limit(S/N=3)was 0.33-3.30μg/kg,the limit of quantification(S/N=10)was 1.0-10.0μg/kg.High-performance liquid chromatography-fluorescence detector-two-stage array tube detection method is suitable for the analysis of PAHs in mutton skewers.

关 键 词：多环芳烃 羊肉串 高效液相色谱-荧光检测器-二级阵列管检测器 分子印迹固相萃取柱 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程] O657.3[轻工技术与工程—食品科学与工程]