摘要
取匀浆后的蔬菜样品5.000g,加入甲酸-乙腈(1+99)混合液10.0 mL,振荡提取20min,加入氯化钠2.0g,继续振荡20min,离心5min。分取上清液1.5mL,加入由N-丙基乙二胺100mg、十八烷基硅烷100 mg和自制的磁化碳纳米管10 mg混合组成的净化剂进行QuEChERS提取净化,混合物经0.22μm滤膜过滤。滤液供高效液相色谱-串联质谱法分析。色谱分离中,选用Waters Cortects C18色谱柱为固定相,以不同比例组成的乙腈(A)和5mmol·L-1乙酸铵溶液(B)的混合液为流动相进行梯度洗脱。洗脱液中29种除草剂的残留量按质谱条件进行测定。结果表明:29种除草剂的质量浓度均在5.0～40μg·L-1范围内与对应的峰面积呈线性关系,检出限(3S/N)在0.5～1.5μg·kg-1之间。以空白蔬菜样品为基体,用标准加入法进行回收试验,测得29种化合物的回收率在83.9%～99.7%之间,测定值的相对标准偏差(n=6)在1.3%～5.6%之间。
A portion of 5.000 g of the homogenized and pulpified vegetable sample was taken and extracted by shaking for 20 min with 10.0 mL of a mixture of formic acid and acetonitrile(1+99),2.0 g of NaCl were added to the mixture and the shaking was continued for another 20 min.After centrifuging for 5 min,an aliquot of 1.5 mL of the supernatant was taken and purified by QuEChERS with a powder mixture containing 100 mg each of N-propyl ethylenediamine and octadecyl silane and 10 mg of self-prepared magnetized carbon nanotubes.The mixture was then filtered through 0.22μm filtering membrane,and the filtrate was used for HPLC-MS/MS analysis.In the HPLC separation,Waters Cortects C18 column was selected as stationary phase and mixtures of CH3 CN(A)and5 mmol·L^-1 CH3 COONH4 solution(B)with various ratios were used as mobile phase in the gradient elution.Residual amounts of the 29 herbicides in the eluates were determined by MS/MS under the instrumental conditions.As shown by the results,linear relationships between values of peak area and mass concentration of the 29 herbicides in the range of 5.0-40μg·L^-1 were obtained,and the detection limits(3 S/N)in the range of 0.5-1.5μg·kg^-1.Test for recovery by standard addition method was made using a blank vegetable sample as matrix,giving results in the range of 83.9%-99.7%,and RSDs(n=6)ranged from 1.3%to 5.6%.
作者
徐潇颖
刘柱
朱炳祺
梁晶晶
陈万勤
罗金文
XU Xiaoying;LIU Zhu;ZHU Bingqi;LIANG Jinking;CHEN Wanqin;LUO Jinwen(Zhejiang Provincial Institute for Food and Drug Control,Hangzhou 310052,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2019年第4期420-426,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
浙江省基础公益研究计划项目(LGF18C200001)
长三角地区食品安全快速与高通量检测技术开发及数据分析共享平台的建设与应用项目(18395810300)
