摘要
以题示方法测定蔬菜样品中磷胺、倍硫磷、喹硫磷、丙溴磷等4种有机磷农药的残留量。采用硝酸钴和甘氨酸燃烧法制备Co_(3)O_(4)多孔材料,通过粉末X射线衍射仪(XRD)、场发射电子扫描显微镜(FESEM)、吸附比表面测试(BET)、热重分析(TG)对材料进行了表征,结果表明,该净化剂为具有层状疏松多孔结构的尖晶石型Co_(3)O_(4)材料,比表面积为22.054 m~2·g^(-1),Co_(3)O_(4)的质量分数为87.0%。蔬菜样品经切碎、研磨后,分取2.5 g,用甲苯5.0 mL涡旋提取5 min。离心,分取4.0 mL上清液,加入0.07 g Co_(3)O_(4)多孔材料,涡旋净化5 min。离心,分取0.6 mL上清液,过0.22μm滤膜,滤液进入气相色谱仪,在HP-5毛细管色谱柱上用程序升温条件分离,用火焰光度检测器测定。结果显示,Co_(3)O_(4)多孔材料的用量仅为QuEChERS法的百分之一;4种有机磷农药均在15 min内实现了基线分离,磷胺还实现了顺反异构的拆分和分离;标准曲线的线性范围分别为0.032~0.60 mg·L^(-1)(磷胺和丙溴磷)和0.016~0.30 mg·L^(-1)(倍硫磷和喹硫磷),检出限(3S/N)为0.004~0.010 mg·L^(-1)。对空白油麦菜样品进行4个浓度水平的加标回收试验,4种有机磷农药的回收率为89.2%~95.8%,测定值的相对标准偏差(n=6)均不大于7.0%;方法用于11种蔬菜样品的分析,均未检出4种有机磷农药的残留,符合GB 2763-2021的规定。
The residues of the 4 organophosphorus pesticides(phosphamidon,fenthion,quinalphos and profenofos)in vegetable samples were determined by the method mentioned by title.Porous material of Co_(3)O_(4)was prepared by the combustion of Co(NO_(3))_(2)and glycine,and characterized by XRD,FESEM,BET and TG.As found by results,the purifier was spinel-type Co_(3)O_(4)material with layered loose porous structure,its specific surface area was 22.054 m^(2)·g^(-1),and mass fraction of Co_(3)O_(4)was 87.0%.After chopping and grinding,2.5 g of vegetable samples were extracted with 5.0 mL of toluene by vortex.After centrifugation,0.07 g of Co_(3)O_(4)porous material was added into 4.0 mL of supernatant,and the mixture was vortexed for 5 min.After centrifugation,an aliquot(0.6 mL)of the supernatant was taken out and passed through a 0.22μm filter membrane.The filtrate was introduced into the gas chromatography,the 4 pesticides were separated on the HP-5 capillary column with temperature program,and detected by flame photometric detector.It was shown that the amount of porous material of Co_(3)O_(4)was only 1%of that of QuEChERS method.A baseline separation of the 4 organophosphorus pesticides was achieved within 15 min,and the cis-and trans-isomers of phosphamidon were also separated.The linear ranges of standard curves were 0.032-0.60 mg·L^(-1)(for phosphamidon and profenofos)and 0.016-0.30 mg·L^(-1)(for fenthion and quinalphos),with detection limits(3 S/N)of 0.004-0.010 mg·L^(-1).Test for the spiked recovery was made on the blank rapeseed samples at the 4 concentration levels,giving recoveries of the 4 organophosphorus pesticides in the range of 89.2%-95.8%,and RSDs(n=6)of the determined values were not more than 7.0%.The proposed method was applied to the analysis of 11 kinds of vegetable samples,and the residues of the 4 organophosphorus pesticides were not detected,which met the requirements of GB 2763-2021.
作者
操江飞
黄芷莹
韦寿莲
谢春生
陈志胜
姬鸿鹤
冯学璞
CAO Jiangfei;HUANG Zhiying;WEI Shoulian;XIE Chunsheng;CHEN Zhisheng;JI Honghe;FENG Xuepu(School of Enuironmental and Chemical Engineering Zhaoqing University,Zhaoqing 526061,hina;Guangdong Prouincial Key Laboratory of Enuironmental Health and Land Resource,Zhaoqing University,Zhaoqing 526061,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2022年第5期564-569,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
肇庆市科技项目(202004030107)
肇庆学院校级项目(202005)。
