Determination of 29 Residual Herbicides in Vegetables by HPLC-MS/MS with QuEChERS Extraction
摘 要
取匀浆后的蔬菜样品5.000 g,加入甲酸-乙腈(1+99)混合液10.0 mL,振荡提取20 min,加入氯化钠2.0 g,继续振荡20 min,离心5 min。分取上清液1.5 mL,加入由N-丙基乙二胺100 mg、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0.22 μm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5 mmol·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5.0~40 μg·L-1范围内与对应的峰面积呈线性关系,检出限(3S/N)在0.5~1.5 μg·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。
Abstract
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 0.22 μm 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 CH3CN (A) and 5 mmol·L-1 CH3COONH4 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 5.0-40 μg·L-1 were obtained, and the detection limits (3S/N) in the range of 0.5-1.5 μg·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%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201904009
所属栏目 工作简报
基金项目 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)
收稿日期 2018/6/30
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备注徐潇颖,工程师,硕士研究生,研究方向为食品安全与分析技术研究
引用该论文: XU Xiaoying,LIU Zhu,ZHU Bingqi,LIANG Jingjing,CHEN Wanqin,LUO Jinwen. Determination of 29 Residual Herbicides in Vegetables by HPLC-MS/MS with QuEChERS Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(4): 420~426
徐潇颖,刘柱,朱炳祺,梁晶晶,陈万勤,罗金文. QuEChERS提取-高效液相色谱-串联质谱法测定蔬菜中29种除草剂的残留量[J]. 理化检验-化学分册, 2019, 55(4): 420~426
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【2】吴春英,谷风,白鹭,等.超高效液相色谱-三重四极杆质谱联用仪同时测定水中9种二苯醚类除草剂[J].分析试验室, 2015,34(9):1014-1017.
【3】平华,李杨,李冰茹,等.基于分散固相萃取-超高效液相色谱串联质谱法同时测定蔬菜中多种除草剂残留的方法[J].中国农业科学, 2017,50(21):4159-4169.
【4】李娜,李辉,邵辉,等.超高效液相色谱-串联质谱法测定人参中磺酰脲类除草剂残留量[J].色谱, 2011,29(4):346-352.
【5】丁菲,李范珠,储晓刚,等.玉米中9种磺酰脲类除草剂的超高效液相色谱-串联质谱法同时测定[J].分析测试学报, 2011,30(1):53-57.
【6】KANG S, CHANG N, ZHAO Y, et al. Development of a method for the simultaneous determination of six sulfonylurea herbicides in wheat, rice, and corn by liquid chromatography-tandem mass spectrometry[J]. Journal of Agricultural and Food Chemistry, 2011,59(18):9776-9781.
【7】SPRINGER V H, APRILE F, LISTA A G. Determination of sulfonylureas in cereal samples with electrophoretic method using ionic liquid with dispersed carbon nanotubes as electrophoretic buffer[J]. Food Chemistry, 2014,143:348-353.
【8】杨益林,潘艳坤,周玉薇,等.液相色谱-串联质谱法测定甘蔗中10种除草剂的残留量[J].理化检验-化学分册, 2017,53(5):507-511.
【9】张建莹,岳振峰,蔡伊娜,等.超高效液相色谱-串联质谱法测定复杂基质食品中二硝基苯胺类除草剂残留量[J].分析测试学报, 2017,36(4):550-554.
【10】方灵,苏德森,刘文静,等.多壁碳纳米管固相萃取气相色谱-串联质谱法测定乌龙茶及土壤中10种三嗪类除草剂残留[J].农药学学报, 2017,19(5):617-623.
【11】乔丹,刘小静,韩典峰,等.气相色谱-质谱法测定动物源性水产品中16种除草剂[J].渔业科学进展, 2017,38(4):172-179.
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