Name: characterization and application of passive samplers for monitoring of pesticides in water
Uploaded: 2016-08-03T09:00:00
Description: Watch this Scientific Journal Video about Characterization and Application of Passive Samplers for Monitoring of Pesticides in Water at JoVE.com

The Swedish EPA (Naturv&#229;rdsverket) (agreement 2208-13-001) and Centre for Chemical Pesticides (CKB) are gratefully acknowledged for funding this project. We thank M&#228;rit Peterson, Henrik Jernstedt, Emma Gurnell and Elin Paulsson at the OMK-lab, SLU, for skillful assistance with analytical support and supply of pesticide standards.

1.被动采样设计和准备<ol><li> 硅橡胶板 <ol><li>切断的硅橡胶片材英寸（600 mm×600毫米，厚0.5毫米）到使用不锈钢刀和使用不锈钢盲铆钉连接它们（3.2毫米×10毫米为2.5毫米×600毫米和2.5毫米×314毫米条纹）用铆钉枪，以获得2.5毫米×914毫米（表面积=457厘米2，吸着剂的质量= 15.6Hz克，体积共取样的条带大小=22.9厘米3）。 </li></ol></li><li>放置硅橡胶在Soxhlet装置的提取室。加?...

<ol>
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在质量控制方面，作为标准程序，实验室空白，检测（LOD），回收率和重复性的限制进行了检查23。在低浓度水平空白样本中检测到一些农药。检测限被设置为最低点的符合的信号的标准来3.信噪比平均检测限为8.0皮克绝对注入对硅橡胶，1.7皮克绝对为POCIS-A，1.6柱校正曲线上的值皮克绝对的POCIS-B，3.0皮克绝对的SDB-RPS磁盘和1.6皮克绝对对C盘18。所有浓度通过加标校正IS混合物。基于...

农药不断引入到水生环境，并可能对水生生物1的风险。通常由于在流或偶发输入（ 例如 ，沉淀，合并的下水道溢出污水泻湖释放）2的波动进行在水性环境农药监测采用抓斗采样，但是，这种取样技术不能完全解释的浓度的时间变化，3。因此，监测的方法需要与杀虫剂相关的环境风险的更好的估计加以改进。被动采样允许在一段时间以最少的基础设施和低污染物浓度4,5-长时间连续监测。 被动采样已被证明是在地下水6的监测，淡水7-10，废水11和海水12的宝贵工具。除了监控的目的<suP&gt; 13,14，被动采样器也已用于非目标分析15，毒理学试验16,17，并且作为替代sediment-和生物监测18。被动采样水不断积聚的化学品和提供时间加权平均（TWA）的浓度14。污染物的吸收取决于采样速率（R S）和被动采样-水分配系数（K PW），它依赖于被动采样设计，采样器材料，污染物的物理化学性质，和环境条件（ 例如 ，水湍流，温度）13,14,19,20。 详细的视频旨在展示如何校准和应用被动采样器在水中的农药。具体目标包括我），以使用五种不同类型的被动SAMPL的124个别农药进行准备，提取和仪器分析器，包括硅橡胶，极性有机化学综合采样（POCIS）-A，POCIS-B，SDB-RPS和C 18磁盘，ⅱ）以评估R 5和K PW用于在实验室摄取研究的杀虫剂，以及iii）来演示如何选择感兴趣和如何计算TWA浓度对于各个被动采样的目标化合物相应的被动采样器。 参考标准和被动采样装置 目标化合物包括124遗留和目前使用的杀虫剂，包括除草剂，杀虫剂和杀真菌剂（ 表1）。内部标准混合物（IS混合物）包括fenoprop（2,4,5-TP），可尼丁-D 3，乙硫磷和特丁-D 5。其他使用的化学品包括甲醇（MeOH），乙腈（ACN），丙酮（ACE）二氯甲烷（DCM），环己烷（CH），乙酸乙酯（EA），石油等她的（PE），2-丙醇，25％氨水溶液，乙酸（醋酸）和甲酸（FA）。五种不同的被动采样装置进行了表征，包括硅橡胶，POCIS-A和POCIS-B，SDB-RPS和C 18盘1,21。 表1.被动采样器的采样率（R&#39;S，L天-1），采样-水分配系数（K&#39;PW，L千克-1），用于浓度的野外样品个别在计算方程（方程） 杀虫剂 。 （从色谱A的1405，卢茨阿伦斯，Atlasi Daneshvar，安娜E.刘珍妮第六，别上五个被动采样器件表征转载于水，1-11版权所有（2015）农药监测，经许可爱思唯尔）22 <a href="https://www.jove.com/files/ftp_upload/54053/Table_1.xlsx" target="_blank">请点击此处下载此文件。</a>

<table border="0" cellpadding="0" cellspacing="0" width="1047">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">Methanol</td>
			<td style="width:164px;">Merck Millipore</td>
			<td style="width:163px;">1.06035.2500</td>
			<td style="width:228px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Acetonitrile</td>
			<td>Merck Millipore</td>
			<td>1.00029.2500&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:22px;width:492px;">Acetone</td>
			<td>Merck Millipore</td>
			<td style="width:163px;">1.00012.2500</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">2-propanol</td>
			<td>Merck Millipore</td>
			<td>1.00272.2500</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Dichloromethane</td>
			<td>Merck Millipore</td>
			<td>1.06054.2500</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Ammoniak</td>
			<td>Merck Millipore</td>
			<td>1.05428.1000</td>
			<td>Purity 25%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Formic acid</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td>94318-50ML-F</td>
			<td>Purity ~98%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:22px;">Ethyl acetate&#160;</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td>31063-2.5L</td>
			<td>for pesticide residue analysis</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:22px;">Petroleum ether&#160;</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td>34491-4X2.5L</td>
			<td>for pesticide residue analysis</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Acetic acid&#160;</td>
			<td style="width:164px;">Sigma-Aldrich</td>
			<td>320099-500ML</td>
			<td>Purity &#8805;99.7%</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Cyclohexane&#160;</td>
			<td style="width:164px;">Fisher Chemicals</td>
			<td>C/8933/17</td>
			<td>for residue analysis</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Empty polypropylene SPE Tube with PE frits, 20 &#956;m porosity, volume 6&#160;mL</td>
			<td style="width:164px;">Supelco</td>
			<td>57026</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">Empore SPE Disks, C18, diam. 47&#160;mm</td>
			<td>Supelco</td>
			<td style="width:163px;">66883-U</td>
			<td>Passive sampler</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">Empore SPE Disks, SDB-RPS (Reversed-Phase Sulfonate), diam. 47&#160;mm</td>
			<td>Supelco</td>
			<td style="width:163px;">66886-U&#160;</td>
			<td>Passive sampler</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">POCIS-A&#160;</td>
			<td>EST</td>
			<td style="width:163px;">POCIS-HLB</td>
			<td>Passive sampler</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">POCIS-B</td>
			<td>EST</td>
			<td style="width:163px;">POCIS-Pesticide&#160;</td>
			<td>Passive sampler</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">Polyethersulfone (PES) membranes</td>
			<td>EST</td>
			<td style="width:163px;">PES</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">Silicone rubber sheet</td>
			<td style="width:164px;">Altec</td>
			<td style="width:163px;">03-65-4516</td>
			<td>Passive sampler</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">Agilent 5975C</td>
			<td style="width:164px;">Agilent Technologies</td>
			<td style="width:163px;">5975C</td>
			<td>GC-MS</td>
		</tr>
		<tr height="23">
			<td height="23" style="height:23px;width:492px;">HP-5MS UI</td>
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			<td style="width:164px;">Phenomenex</td>
			<td style="width:163px;">Strata C18&#8211;E</td>
			<td style="width:228px;">Online SPE column for LC-MS/MS</td>
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			<td height="21" style="height:21px;width:492px;">Strata X, 20 x 2 mm id and 20&#8211;25 &#956;m particle size</td>
			<td style="width:164px;">Phenomenex</td>
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</table>

characterization and application of passive samplers for monitoring of pesticides in water

五种不同的水被动采样进行实验室条件下校准124遗产的测量和当前使用的农药。这项研究提供了被动采样准备，校准，提取方法和仪器分析的协议。采样率（R S）和被动采样水分配系数（K PW）分别计算硅橡胶，极性有机化工综合采样POCIS-A，POCIS-B，SDB-RPS和C 18盘。所选化合物的摄取取决于它们的物理化学性质， 即 ，硅橡胶表现出对更疏水的化合物更好的摄取（登录辛醇-水分配系数（K OW）&gt; 5.3），而POCIS-A，POCIS-B和SDB- RPS盘更适合亲水性化合物（1o9 氏OW &lt;0.70）。

五种不同的被动采样技术124遗产的摄取和当前使用的农药，包括硅橡胶（ 图1），POCIS A，POCIS B，SDB-RPS和C 18盘（ 图2）进行比较。提取方法和仪器分析的性能得到了优化。实验室摄取实验的结果可用于计算R&#39;S和登录K&#39;PW的值的基础上为各个杀虫剂（ 图3）的摄取信息（ 见表1）。?...

Watch this Scientific Journal Video about Characterization and Application of Passive Samplers for Monitoring of Pesticides in Water at JoVE.com

Characterization and Application of Passive Samplers for Monitoring of Pesticides in Water

A protocol about the characterization and application of five different passive sampling devices is presented.

表征和被动采样的应用在农药水监测

Five different water passive samplers were calibrated under laboratory conditions for measurement of 124 legacy and current used pesticides. This study ...

The overall goal of this procedure is to demonstrate preparation, extraction, and analysis of pesticides using five different passive sampling devices and to show how to calibrate them in the laboratory for field application. Passive sampling is a promising tool to answer quick questions for measuring pesticides, continuously at low concentration levels to improve for example, environmental risk assessments. The main advantage of passive sampling is that it's a simple time-integrated method for measuring a broad range of pesticides in aqueous environment.This method is a valuable tool for monitoring of pesticides in water. It can also be used for non-target analyzers, toxicity testing, and as an alternative for sediment and biomonitoring. Following this procedure, sampling rates and passive sampler water partitioning coefficients can be calculated based on the uptake profile for individual pesticides.Cut silicone rubber sheets into stripes of 2.5 millimeters by 600 millimeters and 2.5 millimeters by 214 millimeters using a stainless steel cutter. Connect them using a stainless steel blind rivet with a rivet gun to obtain a total sampler stripe size of 2.5 millimeters by 914 millimeters. After cleaning the silicone rubbers by socket extraction as described in the text protocol attach a silicone rubber stripe to a stainless steel spider sampler holder by wrapping the silicone rubber stripe around the rods on the holder.Attach each end of the silicone rubber stripe to a rod on the holder to the loop at the end of the silicone rubber stripe. For POCIS A place 220 milligrams of HLB bulk sorbent between 2 9.0 centimeters by 9.0 centimeters square PES membranes. For POCIS B, place 220 milligrams of a sorbent mixture between two PES membranes.Compress the sorbent and the two PES membranes between two stainless steel rings manually, and secure onto a stainless steel sample holder. Next, place the SDBRPC and C18 disks between two PES membranes. Similarly compress the disks and two PES membranes between two stainless steel rings manually and secure onto a stainless steel sample holder.Fill the three tanks with natural water. Perform all experiments at a constant water temperature and under turbulent water conditions using two electric pumps attached to the tank wall on each side. Also perform the experiments in the dark to minimize the effect of photo-degradation.Next spike each glass container with a pesticide standard mixture containing 124 pesticides using a glass syringe. Conduct the uptake study in rectangular 95 liter glass containers. Designate tank one for silicone rubber, tank two for POCIS A, POCIS B.And tank three for SDB-RPS disk C18 disk.Take out the passive samplers manually from the tanks at time intervals of 5, 11, 20, and 26 days to determine the sampling rates of the pesticides. In addition, monitor the concentrations of the pesticides in each tank by collecting 100 milliliter water samples at day 0, 5, 11, 20, and 26. Prior to extraction, dry the silicone rubber stripe under a stream of high purity nitrogen gas.For gas chromotography mass spectrometry analysis, carry out the solid liquid extraction using sockslet extraction. After placing the silicone rubber into the sockslet extractor add 250 milliliters petroleum ether and acetone and 3 boiling stones into the round bottom flask. Spike the silicone rubber with 100 microliters of an internal standard mixture using a pipet.Then add 50 milliliters of petroleum acetone into the sockslet extractor. Switch on the heater and run the sockslet extraction for 19 hours and then switch off the heater. Concentrate the extracts by rotory evaporation followed by gentle nitrogen blowdown to one milliliter.Exchange the solvent to 90 to 10 cyclohexane to acetone by adding 3 times 1 milliliter of cyclohexane acetone during the nitrogen blowdown to 1 milliliter. For liquid chromotography tandem mass spectrometry analysis the silicone rubber is extracted with 300 milliliters of methanol. Exchange the solvent to a acetonitrile by adding one milliliter of acetonitrile during the nitrogen blowdown to one milliliter.Open the POCIS sampler carefully and transfer the sorbent with ultra-pure water using a funnel into a pre-cleaned empty polypropylene solid face extraction cartridge containing two polyethylene frets. Dry the sorbent by vacuum to remove water. Prior to elution, spike the sorbent with 100 microliters of an internal standard mixture using a pipet.Elude the POCIS A and POCIS B cartridges using 1.5 milliliters of methanol followed by 8 milliliters of 80 to 20 dychloromethane to methanol for LCMSMS analysis. Concentrate the extracts to 1 milliliter by gentle nitrogen blowdown before exchanging the solvent to acetonitrile by adding 1 milliliter of acetonitrile during the nitrogen blowdown to 1 milliliter. For gas chromotography mass spectrometry analysis POCIS A and B is eluded using 5 milliliters of ethyl acetate and the solvent is exchanged to 90 to 10 cyclohexane to acetone by adding 3 times 1 milliliter of cyclohexane to acetone during the nitrogen blowdown to 1 milliliter.Transfer individual disks of SDB-RPS and C18 into a glass beaker and dry them under nitrogen gas. Spike the disks with 100 microliters of an internal standard mixture using a pipet. Sonicate the disks two times in a glass beaker at room temperature.First with five milliliters of ethyl acetate for ten minutes and then with three milliliters of ethyl acetate for ten minutes. Transfer both extracts into one glass tube before concentrating them to two milliliters by gentle nitrogen blowdown. Split the samples into two one millimeter fractions for GCMS and LCMSMS analysis.In one fraction concentrate the extracts to 0.5 milliliters by gentle nitrogen blowdown and then exchange the solvent to cyclohexane and acetone for GCMS analysis. For LCMSMS analysis concentrate the extracts to 0.5 milliliters by gentle nitrogen blowdown and exchange the solvent to acetonitrile. Shown here are exemplary results for the uptake of acetamiprid in silicone rubber in nanograms showing a linear uptake from day 0 to 20 and then a curvilinear uptake from day 20 to 26.This plot shows exemplary results for the uptake of dimethoate in silicone rubber in nanograms. Showing a linear uptake from day 0 to 10 and then an equilibrium after day 10. The five tested passive samplers were capable of accumulating pesticides with a wide range of different octenol water partition coefficients showing that silicone rubber is more suitable for hydrophobic compounds, whereas more polar compounds were better taken up by POCIS A, POCIS B, and SDB-RPS disk.After watching this video you should have a good understanding how to prepare, extract, and analysis pesticides using five different passive sampling devices and how to calibrate them in the laboratory. While attempting this procedure it's important to remember that this study was performed under static conditions while future uptake study should consider using follow-through exposure or in calibration. The usage of performance compounds, which are spiked to the passive sampler before deployment can be used to calculate n-zeto sampling rates and allow for more accurate estimates of time-rate average concentration.Please don't forget, working with organic solvents acets and basics can be extremely hazardous and precautions like lab coat, gloves, eye protection, should be taken while performing this procedure.

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