基于铁(Ⅲ)-硝基-萨洛芬配合物的共振光散射光谱法测定油茶籽油和自来水中久效磷的含量  

Determination of Monocrotophos in Camellia Seed Oil and Tap Water by Resonance Light Scattering Spectrometry Based on Iron(Ⅲ)-Nitro-Salophen Complex

作　　者：杨静 李倩 任静 聂长明[2] 廖力夫[2] 肖锡林[2,3] YANG Jing;LI Qian;REN Jing;NIE Changming;LIAO Lifu;XIAO Xilin(Hengyang Market Supervision&Inspection and Testing Center,Hengyang 421001,China;Hunan Province Key Laboratory for the Design and Application of Actinide Complexes,School of Chemistry and Chemical Engineering,University of South China,Hengyang 421001,China;Department of Public Health and Laboratory Science,Hengyang Medical School,University of South China,Hengyang 421001,China)

机构地区：[1]衡阳市场监督检验和检测中心,衡阳421001 [2]南华大学化学化工学院湖南省锕系配合物设计与应用重点实验室,衡阳421001 [3]南华大学衡阳医学院公共卫生与检验科学系,衡阳421001

出　　处：《理化检验（化学分册）》2024年第1期38-43,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金项目(1475079);衡阳市科技计划项目(202002032548,202150084066);南华大学大学生创新创业训练计划项目(410)。

摘　　要：提出了基于铁(Ⅲ)-硝基-萨洛芬(I-N-Sal)配合物的共振光散射光谱法测定油茶籽油和自来水中久效磷含量的方法。分别取适量的5-硝基水杨醛和邻苯二胺的乙醇溶液,于40℃水浴回流0.5 h,然后在搅拌条件下加入一定量的九水合硝酸铁的乙醇溶液,反应4 h后,过滤、干燥得到深橙红色固体粉末。紫外-可见吸收光谱、傅里叶变换红外光谱、元素分析、核磁共振氢谱等表征结果显示,制备的产物为四齿席夫碱金属配合物,化学式为C20H12N4O6Fe。在弱碱性条件(pH 8.5)下将0.700μmol·L^(-1)制备的I-N-Sal配合物与久效磷静置反应20 min,形成复合物使体系在300 nm处产生强烈的共振光散射信号。结果表明:I-N-Sal配合物对久效磷表现出较好的选择性;久效磷浓度在0.100~1.100μmol·L^(-1)内与对应的共振光散射强度呈线性关系,检出限(3s/k)为30 nmol·L^(-1);方法用于实际油茶籽油和自来水样品中久效磷的测定,所得结果与NY/T 761-2008的基本一致,并且久效磷的加标回收率为97.0%~103%,测定值的相对标准偏差(n=6)为1.5%~3.8%。A method for the determination of monocrotophos in camellia seed oil and tap water by resonance light scattering spectrometry based on iron(Ⅲ)-nitro-Salophen(I-N-Sal)complex was proposed.The appropriate amounts of ethanol solutions containing 5-nitrosalicylaldehyde and o-phenylenediamine were taken respectively.The mixture were refluxed in water bath at 40℃for 0.5 h,and then a certain amount of ethanol solution containing ferric nitrate nonahydrate was added under the condition of stirring.After reaction for 4 h,the solution was filtrated and dried,and the deep orange-red solid powder was obtained.As shown by the results of UV-Vis spectrometry,Fourier transform infrared spectroscopy,elemental analysis and hydrogen nuclear magnetic resonance spectroscopy,the prepared product was tetradentate Schiff base metal complex,and its chemical formula was C_(20)H_(12)N_4O_6Fe.The prepared I-N-Sal complex(0.700μmol·L^(-1))was reacted with monocrotophos for settling 20 min under the condition of weakly alkaline(pH 8.5),and the formed complex made the system produced strong resonance light scattering signal at 300 nm.It was shown that the I-N-Sal complex showed good selectivity for monocrotophos,and linear relationship between the concentration of monocrotophos and the corresponding resonance light scattering intensity was kept in the range of 0.100-1.100μmol·L^(-1),with detection limit(3s/k)of 30 nmol·L^(-1).The method was applied to the determination of monocrotophos in camellia seed oil and tap water samples,it was shown that the results were basically consistent with those obtained by NY/T 761-2008,and the spiked recoveries of monocrotophos were in the range of 97.0%-103%,with RSDs(n=6)of the determined values ranged from 1.5%to 3.8%.

关 键 词：共振光散射光谱法 四齿席夫碱金属配合物 萨洛芬 久效磷 

分 类 号：O657.3[理学—分析化学]