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1.
建立了猪肉中除虫脲、氟幼脲、杀铃脲、氟铃脲、氟酰脲、氟苯脲、虱螨脲、啶蜱脲、氟虫脲、氟啶脲10种苯甲酰脲类杀虫剂药物残留量测定的高效液相色谱-电喷雾串联质谱方法。样品采用丙酮-正己烷提取,经中性氧化铝固相萃取柱净化,高效液相色谱-电喷雾串联质谱仪多反应监测,外标法定量和质谱确证。10种苯甲酰脲类杀虫剂在5~200μg/L范围内响应与浓度的线性关系良好,相关系数均大于0.9984;检测低限为5.0μg/kg;回收率范围为57.6%~110.0%,相对标准偏差在2.8%~12%(n=6)之间。方法满足国际上对苯甲酰脲类杀虫剂类药物最大残留限量的分析要求,已应于猪肉中苯甲酰脲类杀虫剂残留的检测。  相似文献   

2.
建立了大豆和玉米中苯甲酰脲类农药的反相高效液相色谱-电喷雾串联质谱(LC-ESIMS/MS)检测方法。样品经含0.1%乙酸的乙腈提取、浓缩,阳离子固相萃取柱净化,液相色谱串联质谱测定。9种苯甲酰脲类农药在5.0~200μg/L范围内线性关系良好(r20.995)。在大豆和玉米基质中的检出限均为3.0μg/kg,定量下限均为10.0μg/kg。在10.0、20.0、50.0μg/kg 3个加标水平下,9种苯甲酰脲类农药的回收率为46%~92%,精密度(RSD)小于14%。方法准确、灵敏、简单,适用于大豆和玉米中9种苯甲酰脲类农药残留的同时测定。  相似文献   

3.
建立了果汁蔬菜中8种苯甲酰脲类(杀虫脲、氟苯脲、氟虫脲、氟啶脲、除虫脲、氟铃脲、灭幼脲、氟丙氧脲)农药残留量的液相色谱-电喷雾串联质谱(LC-ESI MS/MS)测定方法。样品用乙腈提取后无需净化,经盐析过滤并以水稀释(1∶1)后,经Waters Atlantis(d C18色谱柱分离,5 mmol/L乙酸铵水溶液和乙腈梯度洗脱,以电喷雾电离串联质谱在负离子多反应监测(MRM)模式下进行测定并确证,外标法定量。8种苯甲酰脲类农药在1.0~100μg/L范围内线性良好,相关系数为0.990 0~0.999 9。对8种农药在毛豆基质中3个添加水平下的回收率进行测定,平均回收率为92%~110%,相对标准偏差为5.5%~12%。方法的检出限(S/N=3)为0.04~0.42μg/kg,定量下限(S/N=10)为0.2~1.5μg/kg。  相似文献   

4.
建立了同时测定蔬菜中氯吡苯脲、除虫脲、灭幼脲、杀铃脲、氟铃脲、氟丙氧脲、氟苯脲、氟啶蜱脲、氟虫脲、丁醚脲、氟啶脲11种苯甲酰脲类农药残留的液相色谱-串联质谱分析方法.试样经乙腈提取,N-丙基乙二胺(PSA)和C18填料分散固相萃取净化,C18柱反相液相色谱分离,以甲醇-0.005 mol/L醋酸铵溶液为流动相梯度洗脱,电喷雾负离子模式离子化,多反应监测方式监测,三重四极杆质谱测定.结果表明:试样中添加10、20、50 μg/kg的11种苯甲酰脲类农药,回收率为69% ~109%,相对标准偏差小于16%(n=5).该方法操作简便、稳定性好、灵敏度高,检出限(LOD)为3 μg/kg,定量下限(LOQ)为10 μg/kg.  相似文献   

5.
建立了蔬菜中虫酰肼和甲氧虫酰肼的高效液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)检测方法。样品经碱性乙腈提取,固相萃取净化,反相高效液相色谱柱分离后进行质谱分析。在选择反应监测模式(SRM)下进行特征母-子离子对信号采集。分别以碎片离子m/z297和m/z149进行外标法定量。虫酰肼和甲氧虫酰肼残留的检出限(S/N=3)为1.0μg/kg,加标回收测得定量限为4.0μg/kg;在5.0~200μg/L时峰强度与质量浓度的线性关系良好(r2>0.996)。在4.0、10.0和20.0μg/kg3个添加水平,通过基质曲线校正后,虫酰肼和甲氧虫酰肼的平均回收率范围为90%~110%和70%~80%;相对标准偏差小于8%。结果表明,该法简单、灵敏,适用于蔬菜中虫酰肼和甲氧虫酰肼残留的分析确证。  相似文献   

6.
提出了高效液相色谱-串联质谱法测定水果中7种苯甲酰脲类杀虫药(除虫脲、灭幼脲、杀铃脲、氟铃脲、氟苯脲、氟虫脲和氟啶脲)残留量的方法。该方法采用多反应监测(MRM)负离子扫描模式,可一次对水果中7种苯甲酰脲类杀虫药进行准确的定性和定量分析;样品用石油醚提取,提取液经分取、水浴45℃氮气吹干、溶解后进行分析。除虫脲、灭幼脲、杀铃脲、氟虫脲和氟啶脲的测定下限(10S/N)为2μg.kg-1,氟铃脲和氟苯脲测定下限(10S/N)为0.5μg.kg-1。7种苯甲酰脲类杀虫药在100μg.kg-1以内呈线性。方法在3个水平的加标回收率在83.8%~94.4%之间,日内相对标准偏差在3.12%~7.43%之间,日间相对标准偏差在3.96%~7.63%之间。  相似文献   

7.
采用溶剂热法制备了磁性金属有机骨架吸附剂Fe_3O_4-NH_2@MIL-101,通过电子显微镜、红外光谱、X射线衍射对吸附剂的形貌和组成进行了表征,磁强计对吸附剂的磁强度进行了测定。使用该吸附剂进行磁固相萃取,结合高效液相色谱-紫外检测,对农田灌溉水中4种苯甲酰脲类杀虫剂(氯吡脲、氟幼脲、氟铃脲和虱螨脲)进行分析。实验对吸附和洗脱条件进行了优化,包括吸附剂用量、吸附时间、pH值、离子强度、洗脱溶剂种类以及洗脱时间和体积。在最佳实验条件下,方法能够有效富集灌溉水中的苯甲酰脲类杀虫剂。4种苯甲酰脲类杀虫剂在0. 010~3. 0 mg/L浓度范围内线性关系良好,相关系数(r)均大于0. 999 5,检出限为0. 03~0. 09μg/L,定量下限为0. 10~0. 30μg/L。方法的加标回收率为81. 7%~95. 4%,RSD小于10%。该方法前处理操作简便,萃取用时不超过15 min,可用于农田灌溉水中苯甲酰脲类杀虫剂的检测。  相似文献   

8.
建立了高效液相色谱-串联质谱(HPLC-MS/MS)法,结合溶剂提取和固相富集技术同时测定茶汤中氟啶脲、除虫脲、啶蜱脲、氟虫脲、氟铃脲、伏虫隆和杀铃脲7种苯甲酰农药残留的方法。研究了提取溶剂的种类、用量和提取时间,以及固相富集小柱的固定相和流动相对7种苯甲酰脲类农药的提取率、分离度、灵敏度和重现性等的影响。结果表明,在最佳条件下,7种苯甲酰脲类农药在6.5min内被完全分离。7种苯甲酰脲类农药残留的检测限(DL)和定量限(QL)分别为0.08~1.00ng/mL和0.09~3.02ng/mL,加标回收率为90%~105%,相对标准偏差(RSD)小于7%(n=6)。利用所建立的方法成功测定了不同茶汤中上述7种苯甲酰脲类农药残留。该方法具有耗时短、灵敏度高、稳定性好等优点,有助于茶叶安全饮用的准确评价。  相似文献   

9.
钱鸣蓉  章虎  吴俐勤  陈志民  王祥云 《色谱》2010,28(9):854-858
建立了同时分析葱中5种双酰肼农药的高效液相色谱-串联质谱方法。样品经乙腈高速匀浆提取,盐析后浓缩,弗罗里硅土柱色谱净化,采用液相色谱-串联质谱分析5种化合物。质谱分析采用电喷雾电离,正离子扫描,多反应监测模式。对双酰肼农药主要碎片的裂解方式进行了剖析。实验证明,柱净化后无明显的基质效应,样品中添加0.002~0.2 mg/kg的5种双酰肼,其回收率为72.6%~95.5%,相对标准偏差(n=5)小于15%;检出限为0.5 μg/kg,定量限为2 μg/kg。该方法提取效果好,具有良好的灵敏度、回收率和重复性。  相似文献   

10.
建立了超高效液相色谱-串联质谱法同时检测土壤中13种磺酰脲类除草剂多残留量的方法。样品经磷酸缓冲液(pH7.8)-甲醇(体积比1∶1)振荡提取,Oasis HLB固相萃取小柱净化后,采用多反应监测模式测定,外标法定量。13种磺酰脲类除草剂在5~200μg/L范围内线性关系良好,相关系数为0.999 1~0.9999。13种除草剂在5、20μg/kg水平下的平均加标回收率为89%~103%,相对标准偏差为1.1%~11.2%。方法的检出限(S/N=3)为0.020~0.092μg/kg,定量下限(S/N=10)为0.07~0.31μg/kg。  相似文献   

11.
Simultaneous determination of pyrethroid, organophosphate (OP) and organochlorine (OC) pesticides in water was achieved with headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-electron-capture detection (GC-ECD). The parameters affecting HS-SPME of pesticides from water were optimized, including extraction temperature, sample and headspace volumes, and sodium chloride amounts. The effects of desorption temperature, desorption time, and position of the fibre in the GC inlet were also investigated. Extraction temperature was the most important factor affecting the recoveries of analytes, and the optimized temperature was 96°C. The addition of salt did not increase extraction efficiencies of the pesticides from the water. The optimized desorption conditions in the GC were as follows: desorption time of 10?min; desorption temperature of 260°C; and a 2?cm position of the fibre in the inlet. The method detection limits were in the low-ng/L level with a linearity range of 50–1000?ng/L for the OCs, 50–5000?ng/L for the OP, and 50–20?000?ng/L for the pyrethroids. These data demonstrated that HS-SPME is a sensitive method for the determination of pyrethroid, OC, and OP pesticides in water.  相似文献   

12.
Gas chromatography-mass spectrometry (GC-MS) with electron impact (EI), positive-ion chemical ionization (PCI) and negative-ion chemical ionization (NCI) were applied as confirmatory techniques for residue analysis of chlorotriazine pesticides, their degradation products and organophosphorus pesticides in soil samples. Clean-up was effected using a Florisil column with subsequent analysis by GC with a nitrogen-phosphorus detector. GC-MS with the EI mode of operation is the common mode of confirmation for all the pesticides. Further confirmation by either GC-MS with PCI and NCI for chlorotriazines and organophosphorus pesticides, respectively, is recommended. The method was applied to the determination of residue levels of atrazine, deethylatrazine, deisopropylatrazine, simazine, fenitrothion and tetrachlorvinphos in several soil samples at levels from 5 ng g?1 to 9 μg g?1.  相似文献   

13.
Abstract

A supercritical fluid extraction (SFE) method was developed for the extraction of 21 organochlorine (OC) pesticides from soil using dichloromethane as cosolvent and magnesium sulfate as drying agent. Average recoveries of spiked OCs from six different soils generally ranged from 70 to 95%, with an average replicate precision of ± 13%. For the extraction of two soils containing “native” OCs, the SFE method gave generally similar or higher concentrations compared to Soxhlet extraction. The precision of replicate analyses of native OCs using SFE and Soxhlet extraction was ± 0.009 and ± 0.007 ug/g, with 24 and 13 degrees of freedom respectively.  相似文献   

14.
A fast separation based on cation‐exchange liquid chromatography coupled with high‐resolution mass spectrometry is proposed for simultaneous determination of chlormequat, difenzoquat, diquat, mepiquat and paraquat in several food and beverage commodities. Solid samples were extracted using a mixture of water/methanol/formic acid (69.6:30:0.4, v/v/v), while liquid samples were ten times diluted with the same solution. Separation was carried out on an experimental length‐modified IonPac CS17 column (2 × 15 mm2) that allowed the use of formic acid and acetonitrile as mobile phase. Detection limits for food and beverage matrices were established at 1.5 μg/L for chlormequat, difenzoquat and mepiquat, and 3 μg/L for diquat and paraquat, while for drinking water a pre‐analytical sample concentration allowed detection limits of 9 and 20 ng/L, respectively. Precision, as repeatability (RSD%), ranged from 0.2 to 24%, with a median value of 6%, and trueness, as recovery, ranged from 64 to 118%, with a median value of 96%. The method developed was successfully applied to investigate the presence of herbicide residues in commercial commodities (mineral water, orange juice, beer, tea, green coffee bean, toasted coffee powder, cocoa bean, white corn flour, rice and sugar samples).  相似文献   

15.
Zhao H  Jia Y  Ding M  Sun D  Zhao M 《色谱》2011,29(5):443-449
建立了多壁碳纳米管为吸附剂的固相萃取(SPE)净化、气相色谱-电子捕获检测(GC-ECD)测定蔬菜中6种有机氯和7种拟除虫菊酯农药的方法。采用双柱(HP-50和HP-1色谱柱)双检测器进行定性和定量分析。蔬菜样品采用乙腈提取,多壁碳纳米管SPE柱净化,正己烷溶解上样,丙酮-正己烷(7:3, v/v)洗脱,13种农药中有11种农药的添加回收率高于70%。将该净化方法用于荷兰黄瓜、卷心菜、红圣女果、奶油生菜、紫甘蓝、韭菜、大葱和洋葱等样品的净化,与弗罗里硅土SPE柱相比较,净化效果更好,表明多壁碳纳米管具有较强的吸附去除色素的能力,可以避免色素对测定的干扰。  相似文献   

16.
Summary A gas chromatographic method employing a capillary column and a selective nitrogen/phosphorus detector (NPD) has been developed for the determination of organophosphorus (OP) and organonitrogen (NP) pesticides in horticultural samples (apples). The separation of sixteen pesticides and the internal standard was performed in thirteen minutes. The analytical characteristics of the method, including linear response ranges, detection limits, and reproducibility, have been studied using a 11 mixture of ethyl acetate and xylene as extraction solvent. The possibility of mutual interference between pesticides has also been studied. A procedure for the quantitative extraction of the sixteen pesticides from apple samples has also been developed; for fifteen of the pesticides recoveries >85% were obtained after 90 minutes extraction. The effect of different solvents both on recovery and on the sensitivity of the subsequent chromatography were also investigated. It was found that the sensitivity required must be considered when the solvent for sample treatment is selected.  相似文献   

17.
The reduction reaction of imidacloprid [1-(6-chloro-3-pyridylmethyl)-N-nitroimidazolidin-2-ylideneamine] at a mercury electrode shows two well-defined waves in the range of pH 2.0–11.0. The characteristics of the electrode processes were examined. The analyte captures four electrons in the first step and two in the second to give the hydroxylamine and amine derivatives, respectively. A differential-pulse polarographic method for the determination of imidacloprid based on the first reduction peak of this compound is presented. Britton-Robinson buffer was used as a supporting electrolyte and optimum pH value was found to be pH 8.O. The applicable concentration range was from 10 to 200 ng/ml, with a relative standard deviation of 1.5% (for a level of 80 ng/ml) and a detection limit of 3 ng/ml. The method has been satisfactorily applied to the determination of imidacloprid in commercial formulations.  相似文献   

18.
The European Union specificies that drinking water can contain pesticide residues at concentrations of up to 0.1 μg/L each and 0.5 μg/L in total, and that 1–3 μg/L of pesticides can be present in surface water, but the general idea is to keep discharges, emissions and losses of priority hazardous substances close to zero for synthetic substances. Therefore, in order to monitor pesticide levels in water, analytical methods with low quantification limits are required. The method proposed here is based on solid phase extraction (SPE) followed by gas chromatography with a nitrogen–phosphorous detector (GC-NPD). During method development, six organophosphate pesticides (azinphos-ethyl, chlorfenvinphos, chlorpyriphos, ethoprophos, fenamiphos and malathion) and two organonitrogen pesticides (alachlor and deltamethrin) were considered as target analytes. Elution conditions that could influence the efficiency of the SPE were studied. The optimized methodology exhibited good linearity, with determination coefficients of better than 0.996. The analytical recovery for the target analytes ranged from 70 to 100%, while the within-day precision was 4.0–11.5 %. The data also showed that the nature of the aqueous matrice (ultrapure, surface or drinking water) had no significant effect on the recovery. The quantification limits for the analytes were found to be 0.01–0.13 μg/L (except for deltamethrin, which was 1.0 μg/L). The present methodology is easy, rapid and gives better sensitivity than solvent drop microextraction for the determination of organonitrogen and organophosphate pesticides in drinking water at levels associated with the legislation.  相似文献   

19.
醚型菊酯类农药通用抗原的合成及鉴定   总被引:1,自引:0,他引:1  
以2-(4-乙氧基苯基)-2-甲基丙醇和氯乙酸钠为原料,合成了醚型菊酯类农药通用半抗原Hapten I,经1 H-NMR及13C-NMR鉴定后,分别与牛血清蛋白(BSA)和卵清白蛋白(OVA)偶联,制得免疫原和包被原,经紫外光谱分析法计算得其偶联比分别为14∶1和35∶1,说明人工抗原合成成功.免疫Balb/c小鼠制备多克隆抗体,效价达1.28×105,用半抗原经间接竞争ELISA检测人工抗原的免疫原性,IC50和IC10值分别为0.2653和0.0012 mg/L,证明人工抗原具有较好的免疫原性.交叉反应表明此多克隆抗体具有良好的特异性.  相似文献   

20.
多壁纳米碳管固相萃取测定水中的有机氯农药   总被引:10,自引:3,他引:7  
对于水样中的有机氯农药的净化方法主要是采用传统的液液分配的方法,缺点是溶剂使用量和前处理复杂。近年来固相萃取及固相微萃取等技术被应用到水样中的有机污染物的测定。如利用键合在硅胶上的非极性(C18,LC18等)或极性物质(LC-CN,LC-NH2)对水中有机物进行富集,用GDX或XAD自填的固相柱的报道也很多。纳米技术和纳米材料的发展为开发固相萃取材料带来新契机。纳米材料是指尺寸大小在从1~100m之间物质。与普通的块体材料相比,纳米材料具有较大的比表面,因而有可能具有较大吸附容量。纳米材料在环境有机污染物分离富集方面的应用研究才刚刚开始。本文主要就纳米碳管对水样中的有机氯农药进行研究,优化固相萃取条件。  相似文献   

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