搜索热:失效分析 陶瓷
扫一扫 加微信
首页 > 期刊论文 > 论文摘要
QuEChERS提取-超高效液相色谱-串联质谱法测定蔬菜中氨基甲酸酯类农药的残留量
          
Determination of Carbamate Pesticides Residues in Vegetables by UPLC-MS/MS with QuEChERS Extraction

摘    要
将蔬菜样品粉碎匀浆后于-20℃保存备用。取此样品10.00 g与含1.3%(体积分数)甲酸溶液的乙腈10 mL充分混匀后超声提取20 min,加入无水硫酸钠8.2 g作为脱水剂,氯化钠3.0 g作为盐析剂,混合后离心5 min。取出上清液并保留。对留下的样品按上述方法重复提取1次。将2次所得上清液合并,并从中分取2.0 mL溶液,加入吸附剂N-丙基乙二胺(PSA)0.4 g,C18 0.25 g和石墨化碳黑(GCB)8.2 mg,涡旋振荡2 min进行净化处理,随即离心2 min,取上清液经0.22 μm滤膜过滤。取滤液,按超高效液相色谱-串联质谱法测定其中6种氨基甲酸酯类农药的残留量。用Agilent Poroshell 120 EC-C18色谱柱为固定相,进样量为5 μL。用由不同比例的(A)20 mmol·L-1乙酸铵溶液(每升中含乙酸1 mL)和(B)乙腈组成混合液作为流动相进行梯度洗脱。串联质谱分析选择电喷雾离子源和多反应监测模式。所测定的6种氨基甲酸酯类农药的工作曲线的线性范围均为0.200~100 μg·L-1,并测得其检出限(3S/N)为0.08~0.38 μg·kg-1。按标准加入法进行回收试验,测得回收率为81.0%~111%,测定值的相对标准偏差(n=6)为2.8%~4.9%。
标    签 QuEChERS提取   超高效液相色谱-串联质谱法   氨基甲酸酯类农药   蔬菜   QuEChERS extraction   UPLC-MS/MS   carbamate pesticide   vegetable  
 
Abstract
Vegetable samples were homogenized and kept at -20℃ separately for use as analytical samples. 10.00 g of the homogenized sample were mixed with 10 mL of a mixture of acetonitrile containing 1.3% (volume fraction) formic acid, and extracted ultrasonically for 20 min. After adding 8.2 g of anhydrous sodium sulfate (as dehydrator) and 3.0 g of sodium chloride (as salting-out agent), the mixture was centrifuged for 5 min. The supernatant was separated and preserved. The sample was extracted once more as described above. The supernatants were combined, and an aliquot of 2.0 mL was taken and purified by swirling with 0.4 g of PSA, 0.25 g of C18 and 8.2 mg of GCB for 2 min, and then centrifuged for 2 min. The supernatant was taken and filtered through 0.22 μm filtering membrane. The filtrate was used as testing solution for determination of residual amounts of the 6 carbamate pesticides by UPLC-MS/MS. In UPLC separation, Agilent Poroshell 120 EC-C18 column was used as stationary phase and mixtures in various ratios of (A) 20 mmol·L-1 NH4OAc solution (containing 1 mL of acetic acid perliter) and (B) acetonitrile were used as mobile phases in programed gradient elution. ESI and MRM mode were adopted in MS/MS. Linear relationships were found between values of peak areas of the 6 carbamate presticides and the respective mass concentrations in the same range of 0.200-100 μg·L-1, with their detection limits (3S/N) in the range of 0.08-0.38 μg·kg-1. Test for recovery was made by standard addition method, giving results in the range from 81.0% to 111%, and values of RSDs (n=6) ranged from 2.8% to 4.9%.

中图分类号 O657.63   DOI 10.11973/lhjy-hx202001010

 
  中国光学期刊网论文下载说明


所属栏目 工作简报

基金项目 淮安市科技局科技支撑(社会发展)项目(HAS2015030);江苏省卫生计生委预防医学科研项目(Y2018048)

收稿日期 2019/6/4

修改稿日期

网络出版日期

作者单位点击查看


备注杭学宇,主任技师,主要从事卫生检验工作

引用该论文: HANG Xueyu,WU Junwei,SONG Xin,WANG Qin,FENG Xiaoqing,WANG Lu,XU Rui,WANG Dandan,LU Juan. Determination of Carbamate Pesticides Residues in Vegetables by UPLC-MS/MS with QuEChERS Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(1): 60~65
杭学宇,吴珺玮,宋鑫,王芹,冯晓青,王露,徐瑞,王丹丹,陆娟. QuEChERS提取-超高效液相色谱-串联质谱法测定蔬菜中氨基甲酸酯类农药的残留量[J]. 理化检验-化学分册, 2020, 56(1): 60~65


论文评价
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
分享论文
分享到新浪微博 分享到腾讯微博 分享到人人网 分享到 Google Reader 分享到百度搜藏分享到Twitter

参考文献
【1】FUKUTO T R. Mechanism of action of organophosphorus and carbamate insecticides[J]. Environmental Health Perspectives, 1990,87:245-254.
 
【2】COSTA C, CATANIA S, SILVARI V. Genotoxicity and activation of organophosphate and carbamate pesticides by cytochrome P4502D6[J]. Giornale Italiano Di Medicina Del Lavoro ed Ergonomia, 2003,25(S3):81-82.
 
【3】王小平,王鹏,朱蔚.急性有机磷混合氨基甲酸酯农药中毒7例治疗体会[J].现代中西医结合杂志, 2007,16(28):4192-4193.
 
【4】FERNÁNDEZ M, PICÓ Y, MAÑES J. Determination of carbamate residues in fruits and vegetables by matrix solid-phase dispersion and liquid chromatography-mass spectrometry[J]. Journal of Chromatography A, 2000,871:43-56.
 
【5】GOULART S M, ALVES R D, NEVES A A, et al.Optimization and validation of liquid-liquid extraction with low temperature partitioning for determination of carbamates in water[J]. Analytica Chimica Acta, 2010,671(1/2):41-47.
 
【6】ROSSI S, DALPERO A P, GHINI S, et al. Multiresidual method for the gas chromatographic analysis of pesticides in honeybees cleaned by gel permeation chromatography[J]. Journal of Chromatography A, 2001,905(1/2):223-232.
 
【7】宋鑫,王芹,杭学宇,等.全自动GPC-SPE-UPLC-MS/MS检测中药饮片中氨基甲酸酯类农药残留[J].中国药师, 2017(12):2165-2168.
 
【8】ANASTASSIADES M, LEHOTAY S J, STAJNBAHER D, et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce[J]. Journal of AOAC International, 2003,86(2):412-431.
 
【9】NANTIA E A, MORENOGONZALEZ D, MANFO F P, et al. QuEChERS-based method for the determination of carbamate residues in aromatic herbs by UHPLC-MS/MS[J]. Food Chemistry, 2017,216:334-341.
 
【10】王连珠,周昱,陈泳,等.QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估[J].色谱, 2012,30(2):146-153.
 
【11】MASTOVSKA K, LEHOTAY S J. Evaluation of common organic solvents for gas chromatographic analysis and stability of multiclass pesticide residues[J]. Journal of Chromatography A, 2004,1040(2):259-272.
 
相关信息
   标题 相关频次
 磁性固相萃取-高效液相色谱法测定葡萄酒中罗丹明B的含量
 12
 气相色谱-质谱法测定生活饮用水中23种有机磷农药的含量
 12
 新型磁性分子印迹聚合物快速萃取-高效液相色谱法测定牛血清白蛋白
 12
 自制四氧化三锰纳米粒子固相萃取-电感耦合等离子体质谱法测定蔬菜中铅和铜
 12
 磁性固相萃取-火焰原子吸收光谱法测定工业废水中的Cu2+
 10
 高效液相色谱-串联质谱法测定食用植物油中4-壬基酚的含量
 10
 水和白酒中异味物质检测的研究进展
 10
 用于分离富集己烯雌酚的磁性分子印迹聚合物的制备及其在环境水样检测中的应用
 10
 磁性碳纳米管固相萃取-原子荧光光谱法测定水中痕量镉
 8
 淮安市不同水体中邻苯二甲酸酯的固相萃取-超高效液相色谱-串联质谱法测定及其污染特征研究
 7
 磁性固相萃取-高效液相色谱法测定牛奶中4种磺胺类药物
 6
 水和食品中有机磷农药残留检测的研究进展
 6
 全自动凝胶渗透色谱-固相萃取联合净化-超高效液相色谱-串联质谱法测定肉类制品中8种工业染料
 5
 多壁碳纳米管基质固相分散萃取-高效液相色谱法测定蔬菜中7种氨基甲酸酯类农药残留量
 4
 QuEChERS-超高效液相色谱-串联质谱法同时测定人全血中5种氨基甲酸酯类农药
 3
 QuEChERS前处理结合超高液相色谱-串联质谱法测定高硫蔬菜中16种氨基甲酸酯类农药残留
 3
 超高效液相色谱-串联质谱法测定保健食品中7种非法添加的化学镇静剂
 3
 固相萃取-气相色谱法测定蔬菜中氨基甲酸酯类农药残留
 3
 环境和生物样品中有机氯农药残留检测研究进展
 3
 气相色谱-串联质谱法测定蔬菜和土壤中17种邻苯二甲酸酯
 3
 42CrMo钢轴箱端盖疲劳断裂原因
 2
 QuEChERS-超高效液相色谱-串联质谱法快速测定鱼肉中22种磺胺类药物残留
 2
 QuEChERS净化-超高效液相色谱-串联质谱法测定茶叶中吡虫啉和噻嗪酮的残留量
 2
 QuEChERS净化-高效液相色谱法测定蔬菜中除虫脲和灭幼脲的残留量
 2
 QuEChERS提取-超高效液相色谱-串联质谱法测定腐败人血中3种钩吻生物碱
 2
 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
 2
 QuEChERS提取-高效液相色谱-高分辨质谱法测定水产品中3种蓝藻毒素的含量
 2
 X65管线钢在模拟海水环境中的腐蚀行为
 2
 超高效液相色谱-串联质谱法测定白芷中51种禁用农药的残留量
 2
 超高效液相色谱-串联质谱法测定纺织品中4种长链全氟烷酸的含量
 2