气相色谱-三重四极杆质谱法测定婴幼儿配方乳粉中24种多环芳烃的含量  

Determination of 24 Polycyclic Aromatic Hydrocarbons in Infant Formula by Gas Chromatography-Triple Quadruple Mass Spectrometry

作　　者：王玮[1] 郭蓉[1] 赵莹 田丽[1] 刘存卫 梁晓聪[1] WANG Wei;GUO Rong;ZHAO Ying;TIAN Li;LIU Cunwei;LIANG Xiaocong(Shaanxi Provincial Center for Disease Control and Prevention,Xi'an 710054,China)

机构地区：[1]陕西省疾病预防控制中心,西安710054

出　　处：《理化检验（化学分册）》2022年第11期1287-1293,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：在样品中加入混合内标溶液、水和氨水,在65℃水浴中加热10min。用无水乙醇、无水乙醚和石油醚萃取,振荡、离心后取上层有机相,于45℃氮吹至干。加入含氢氧化钾的乙醇溶液,于70℃皂化3 min。加入水、正己烷,涡旋、离心,取正己烷相过活化好的EU多环芳烃(PAHs)固相萃取柱,流量控制在1.0mL·min^(-1)左右。用正己烷淋洗固相萃取柱,用体积比1∶1的二氯甲烷-乙酸乙酯混合溶液洗脱。收集洗脱液,于40℃氮吹至干,残留物用体积比1∶1丙酮-异辛烷混合溶液复溶,过0.22μm滤膜。滤液进入气相色谱仪,在DB-EUPAH毛细管色谱柱上进行程序升温分离,分离后的目标物在串联质谱仪中用多反应监测模式检测,内标法定量。结果显示:24种PAHs的质量浓度均在0.244~15.6μg·L^(-1)内与其对应的峰面积及内标峰面积的比值呈线性关系,检出限为0.008~0.200μg·kg^(-1);加标回收率为72.0%~128%,测定值的相对标准偏差(n=6)不大于12%。该方法用于11份市售婴幼儿配方乳粉的分析,阳性样品检出率为45.45%;检出的PAHs为■、苯并[a]蒽、苯并[b]荧蒽、苯并[a]芘,其他20种PAHs均未检出;1份1段婴幼儿配方奶粉中PAHs总检出量(1.92μg·kg^(-1))超过了EC No 835/2011规定的限值(1.00μg·kg^(-1))。The mixed internal standard solution, water and aqueous ammonia were mixed with the sample, and the mixture was heated in the water bath at 65 ℃ for 10 min. Anhydrous ethanol, anhydrous diethyl ether and petroleum ether were added for extraction. After vibration and centrifugation, the upper organic phase was taken and blown to dryness by nitrogen at 45 ℃. Ethanol solution containing potassium hydroxide was added, and the mixture was saponified at 70 ℃ for 3 min. Water and n-hexane were added, and the solution was vortexed and centrifuged, n-hexane phase of which was taken and passed through EU polycyclic aromtic hydrocarbons(PAHs) solid phase extraction column activated at the flow rate around 1.0 mL·min-1. The above column was rinsed with n-hexane, and eluted with the mixed solution of dichloromethane and ethyl acetate at volume ratio of 1∶1. The eluent was collected and blown to dryness by nitrogen at 40 ℃. The residue was redissolved by the mixed solution of acetone and isooctane at volume ratio of 1∶1, and the above solution was passed through a 0.22 μm filter membrane. The filtrate was introduced into the gas chromatograph, and separated on DB-EUPAH capillary column under programed temperature. Targets obtained was detected by multiple reaction monitoring mode in the tandem mass spectrometer, and quantified by internal standard method. It was shown that the mass concentrations of the 24 PAHs were linearly related with the ratios of the respective chromatographic peak area to the peak area of internal standard in the range of 0.244-15.6 μg·L-1, with detection limits in the range of 0.008-0.200 μg·kg-1. The spiked recoveries ranged from 72.0% to 128%, giving RSDs(n=6) of the determined values not more than 12%. The prescribed method was applied to the analysis of 11 commercial infant formulas, and the positive sample detection rate was 45.45%. The PAHs detected were chlorobenzene, benzo [a] anthracene, benzo [b] fluoranthene and benzo [a] pyrene, while the other 20 PAHs were not detected, wi

关 键 词：气相色谱-三重四极杆质谱法 多环芳烃化合物 婴幼儿配方乳粉 

分 类 号：O657.63[理学—分析化学]