摘要
取水样50.0 mL,加盐酸调节pH至3.0,用吡咯烷酮基和二乙烯基苯修饰的磁性纳米材料50.0 mg振荡吸附20 min。乙腈3.0 mL洗脱后,将洗脱液离心5 min,过0.22μm有机滤膜,氮吹至近干,用甲醇-0.1%(体积分数)甲酸(60+40)混合液定容至1 mL。所得溶液进行超高效液相色谱分离,以XDB-C18反相色谱柱为固定相,以不同体积比的甲醇和0.1%(体积分数)甲酸溶液的混合液为流动相梯度洗脱。质谱分析采用多反应监测模式。4种苯脲类除草剂的质量浓度在0.05~5.0μg·L^(-1)内与其峰面积呈线性关系,检出限(3.143s)为12.5~16.4 ng·L^(-1)。按标准加入法进行回收试验,回收率为83.7%~107%,测定值的相对标准偏差(n=6)均小于8.5%。
The sample （50. 0 mL） was adjusted pH to 3. 0 with HC1 solution, and adsorbed by swirling for 20 rain with 50. 0 mg of magnetic nanomaterials modified with ketopyrrolidine and divinylbenzene. After elution with 3. 0 mL of acetonitrile, the eluent was centrifuged for 5 min, and filtered through 0. 22 9m organic filter membrane. The filtrate was dried by N2-blowing, and made up its volume to 1 mL, with a mixture of methanol-0. 1% （φ） formic acid （60 ＋ 40 ）. The sample solution was separated by UHPLC using XDB-C18 reversed-phase chromatographic column as stationary phase, and mixtures of methanol and 0. 1% （φ） formic acid solution in various volumic ratios as mobile phase in gradient elution. MRM was adopted in MS. Linear relationships between values of peak area and mass concentration of 4 pheulurea herbicides were found in the range of 0. 05--5.0 μg · L^-1 , with detection limits （3. 143s） in the range of 12. 5-16. 4 ng · L^-1. Test for recovery was made by standard addition method, giving results in the range of 83.7%-107^, with RSDs （n=6） all less than 8.5%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2018年第1期77-81,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
江苏省高校自然科学研究重大项目(15KJA610003)
苏州科技大学校青年基金(341511201)
作者简介
金晶（1991-），女，江苏南通人，硕士研究生，研究方向为环境污染物分析检测;通信联系人。zhanenzhang@126．com
