超高效液相色谱-串联质谱法测定尿液中118种农药残留
O658; 为有效监测人尿液中的农药多残留水平,为健康风险评估提供重要的技术手段,实验利用QuEChERS前处理方法结合超高效液相色谱-三重四极杆质谱技术建立了尿液中 118 种农药的快速筛查及测定方法.通过对前处理过程、液相色谱分离和质谱条件的系统优化,实现了在 2h内对样品中 118 种目标分析物的提取及分析测定.具体方法如下:尿液样品中农药目标分析物采用乙腈提取,无水MgSO4 加NaCl作除水盐析剂,再以C18、PSA、无水MgSO4 为净化吸附剂,经QuEChERS法净化,氮吹复溶后,以 0.01%甲酸水溶液(含 2 mmol/L甲酸铵)及 0.01%甲酸甲醇溶液(含 2 mmol/...
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Published in | Sepu Vol. 42; no. 1; pp. 52 - 63 |
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Main Authors | , , , , , , , , , |
Format | Journal Article |
Language | Chinese English |
Published |
No. 457, Zhongshan Road, Shahekou District, Dalian City, Liaoning Province
合肥海关技术中心,安徽 合肥 230022%人口健康与优生安徽省重点实验室(安徽医科大学),安徽 合肥 230032
08.01.2024
安徽医科大学公共卫生学院,安徽 合肥 230032%合肥海关技术中心,安徽 合肥 230022%安徽医科大学公共卫生学院,安徽 合肥 230032 人口健康与优生安徽省重点实验室(安徽医科大学),安徽 合肥 230032 Editorial board of Chinese Journal of Chromatography |
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Online Access | Get full text |
ISSN | 1000-8713 1872-2059 |
DOI | 10.3724/SP.J.1123.2023.04001 |
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Abstract | O658; 为有效监测人尿液中的农药多残留水平,为健康风险评估提供重要的技术手段,实验利用QuEChERS前处理方法结合超高效液相色谱-三重四极杆质谱技术建立了尿液中 118 种农药的快速筛查及测定方法.通过对前处理过程、液相色谱分离和质谱条件的系统优化,实现了在 2h内对样品中 118 种目标分析物的提取及分析测定.具体方法如下:尿液样品中农药目标分析物采用乙腈提取,无水MgSO4 加NaCl作除水盐析剂,再以C18、PSA、无水MgSO4 为净化吸附剂,经QuEChERS法净化,氮吹复溶后,以 0.01%甲酸水溶液(含 2 mmol/L甲酸铵)及 0.01%甲酸甲醇溶液(含 2 mmol/L甲酸铵)作为流动相,ZORBAX Eclipse Plus C18柱(100 mm×2.1 mm,1.8 μm)作为分析色谱柱,梯度洗脱分离,超高效液相色谱-三重四极杆质谱正负离子切换动态多反应监测(DMRM)模式检测,外标法定量.结果表明,该方法可以对尿液中的 118 种农药同时进行快速测定,检出限均可达到 0.10 μg/L,定量限均可达到 0.50 μg/L,基质效应均小于 20%.在 0.50、1.00、5.00 μg/L 3 个添加水平下,尿样中 118 种农药残留的平均回收率为 70.2%~104%,相对标准偏差(RSD)为 2.8%~9.3%.采用本方法对 10 份尿液样品进行检测,共检出噻虫嗪、噻虫胺、啶虫脒、呋虫胺、异丙隆、烯酰吗啉 6 种农药,含量均≤3.65 μg/L.检出的农药噻虫嗪、噻虫胺与当前该类农药在农产品中的使用情况关联性较高.该方法高效、灵敏、准确,可用于人尿液样品中 118 种农药残留的快速筛查测定. |
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AbstractList | O658; 为有效监测人尿液中的农药多残留水平,为健康风险评估提供重要的技术手段,实验利用QuEChERS前处理方法结合超高效液相色谱-三重四极杆质谱技术建立了尿液中 118 种农药的快速筛查及测定方法.通过对前处理过程、液相色谱分离和质谱条件的系统优化,实现了在 2h内对样品中 118 种目标分析物的提取及分析测定.具体方法如下:尿液样品中农药目标分析物采用乙腈提取,无水MgSO4 加NaCl作除水盐析剂,再以C18、PSA、无水MgSO4 为净化吸附剂,经QuEChERS法净化,氮吹复溶后,以 0.01%甲酸水溶液(含 2 mmol/L甲酸铵)及 0.01%甲酸甲醇溶液(含 2 mmol/L甲酸铵)作为流动相,ZORBAX Eclipse Plus C18柱(100 mm×2.1 mm,1.8 μm)作为分析色谱柱,梯度洗脱分离,超高效液相色谱-三重四极杆质谱正负离子切换动态多反应监测(DMRM)模式检测,外标法定量.结果表明,该方法可以对尿液中的 118 种农药同时进行快速测定,检出限均可达到 0.10 μg/L,定量限均可达到 0.50 μg/L,基质效应均小于 20%.在 0.50、1.00、5.00 μg/L 3 个添加水平下,尿样中 118 种农药残留的平均回收率为 70.2%~104%,相对标准偏差(RSD)为 2.8%~9.3%.采用本方法对 10 份尿液样品进行检测,共检出噻虫嗪、噻虫胺、啶虫脒、呋虫胺、异丙隆、烯酰吗啉 6 种农药,含量均≤3.65 μg/L.检出的农药噻虫嗪、噻虫胺与当前该类农药在农产品中的使用情况关联性较高.该方法高效、灵敏、准确,可用于人尿液样品中 118 种农药残留的快速筛查测定. 为有效监测人尿液中的农药多残留水平,为健康风险评估提供重要的技术手段,实验利用QuEChERS前处理方法结合超高效液相色谱-三重四极杆质谱技术建立了尿液中118种农药的快速筛查及测定方法。通过对前处理过程、液相色谱分离和质谱条件的系统优化,实现了在2 h内对样品中118种目标分析物的提取及分析测定。具体方法如下:尿液样品中农药目标分析物采用乙腈提取,无水MgSO 4 加NaCl作除水盐析剂,再以C 18 、PSA、无水MgSO 4 为净化吸附剂,经QuEChERS法净化,氮吹复溶后,以0.01%甲酸水溶液(含2 mmol/L甲酸铵)及0.01%甲酸甲醇溶液(含2 mmol/L甲酸铵)作为流动相,ZORBAX Eclipse Plus C 18 柱(100 mm×2.1 mm, 1.8 μm)作为分析色谱柱,梯度洗脱分离,超高效液相色谱-三重四极杆质谱正负离子切换动态多反应监测(DMRM)模式检测,外标法定量。结果表明,该方法可以对尿液中的118种农药同时进行快速测定,检出限均可达到0.10 μg/L,定量限均可达到0.50 μg/L,基质效应均小于20%。在0.50、1.00、5.00 μg/L 3个添加水平下,尿样中118种农药残留的平均回收率为70.2%~104%,相对标准偏差(RSD)为2.8%~9.3%。采用本方法对10份尿液样品进行检测,共检出噻虫嗪、噻虫胺、啶虫脒、呋虫胺、异丙隆、烯酰吗啉6种农药,含量均≤3.65 μg/L。检出的农药噻虫嗪、噻虫胺与当前该类农药在农产品中的使用情况关联性较高。该方法高效、灵敏、准确,可用于人尿液样品中118种农药残留的快速筛查测定。 |
Abstract_FL | Pesticide residues in food and their hazardous effects have attracted much attention given the increased and widespread use of pesticides.The long-term consumption of food con-taining pesticide residues is an important pathway for the gradual accumulation of pesticides in the human body.Urine is often monitored as a biological sample for low-dose exposure to pesti-cides,and urine collection is a relatively convenient sampling technique in general population research.In order to effectively monitor residual levels of multiple pesticides in human urine and provide an important technological approach for health risk assessment,a rapid screening and confirmatory detection method for 118 pesticides in urine was established using QuEChERS method as a pretreatment combined with ultra-high performance liquid chromatography-triple quadrupole mass spectrometry(UHPLC-MS/MS).The 118 pesticides analyzed included organo-phosphorus,carbamate,neonicotinoid,and strobilurin fungicides and other widely used pesti-cides.Following systematic optimization of the pretreatment process,LC separation conditions,and MS/MS parameters,118 pesticides were extracted from urine samples and analyzed within 2 h.In brief,the target analytes in 5 mL urine samples were extracted with 10 mL of acetonitrile and added with 5 g of anhydrous MgSO4 and 1 g of NaCl as water-removal and salting-out agents,respectively.After centrifugation,6 mL of the supernatant was cleaned using the QuEChERS method with 300 mg of C18,300 mg of primary secondary amine(PSA)and 900 mg of anhydrous MgSO4 as the purification adsorbent.After nitrogen blowing and solubilization,the 118 target analytes were separated on a ZORBAX Eclipse Plus C18 analytical chromatographic column(100 mm×2.1 mm,1.8 μm)with gradient elution using(A)0.01%formic acid aque-ous solution(containing 2 mmol/L ammonium formate)and(B)0.01%formic acid methanol solution(containing 2 mmol/L ammonium formate)as mobile phases.The gradient elution pro-gram was as follows:0-0.5 min,5%B;0.5-1.5 min,5%B-20%B;1.5-2.5 min,20%B-50%B;2.5-8.0 min,50%B-80%B;8.0-9.0 min,80%B-98%B;9.0-11.0 min,98%B;11.0-11.5 min,98%B-5%B;11.5-15.0 min,5%B.The analytes were then determined by UHPLC-MS/MS with positive/negative ion switching in dynamic multiple-reaction monitoring mode and quantified using the external standard method.The results indicated that the proposed method can determine 118 pesticides in urine simultaneously and rapidly.The limits of detection and limits of quantification were 0.10 and 0.50 μg/L,respectively,and the matrix effects were less than 20%for all targeted compounds.The recoveries of the 118 pesticides in urine were between 70.2%and 104%at three spiked levels of 0.50,1.00,and 5.00 μg/L,and the relative standard deviations ranged from 2.8%to 9.3%.The method was applied to 10 actual urine samples,and the results revealed the presence of six pesticides,including thiamethoxam,clothianidin,acet-amiprid,dinotefuran,isoproturon,and dimethomorph,with contents ranging from<LOQ to 3.65 μg/L.Thiamethoxam and clothianidin were detected most often in the samples,and their concentrations were highly correlated with the current use of these pesticides in edible agricul-tural products.The proposed method has the characteristics of high efficiency,sensitivity,and accuracy and is suitable for the rapid screening and determination of the 118 pesticide residues in human urine samples. |
Author | 刘开永 周典兵 倪亚超 贾学颖 韩芳 王钰 刘宇欣 胡亚蓉 陈莉君 宋伟 |
AuthorAffiliation | 人口健康与优生安徽省重点实验室(安徽医科大学),安徽 合肥 230032;合肥海关技术中心,安徽 合肥 230022%人口健康与优生安徽省重点实验室(安徽医科大学),安徽 合肥 230032;安徽医科大学公共卫生学院,安徽 合肥 230032%合肥海关技术中心,安徽 合肥 230022%安徽医科大学公共卫生学院,安徽 合肥 230032 |
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Author_FL | SONG Wei LIU Kaiyong ZHOU Dianbing JIA Xueying HU Yarong HAN Fang LIU Yuxin NI Yachao WANG Yu CHEN Lijun |
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DocumentTitle_FL | Determination of 118 pesticide residues in urine by ultra-high performance liquid chromatography-tandem mass spectrometry |
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Keywords | 超高效液相色谱-串联质谱 多残留 pesticides urine multi-residues QuEChERS 尿液 农药 ultra-high performance liquid chromatography-tandem mass spec-trometry(UHPLC-MS/MS) |
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Snippet | O658; 为有效监测人尿液中的农药多残留水平,为健康风险评估提供重要的技术手段,实验利用QuEChERS前处理方法结合超高效液相色谱-三重四极杆质谱技术建立了尿液中 118 种农... 为有效监测人尿液中的农药多残留水平,为健康风险评估提供重要的技术手段,实验利用QuEChERS前处理方法结合超高效液相色谱-三重四极杆质谱技术建立了尿液中118种农药的快速... |
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Title | 超高效液相色谱-串联质谱法测定尿液中118种农药残留 |
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