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. Passive Sampler Design and Preparation
<ol>
	<li>Silicone rubber sheets
	<ol>
		<li>Cut the silicone rubber sheets (600 mm x 600 mm, 0.5 mm thick) into stripes of 2.5 mm x 600 mm and 2.5 mm x 314 mm using a stainless steel cutter and connect them using a stainless steel blind rivet (3.2 mm x 10 mm) with a rivet gun to obtain a total sampler stripe size of 2.5 mm x 914 mm (surface area = 457 cm2, sorbent mass = 15.6 g, volume = 22.9 cm3).</li>
	</ol>
	</li>
	<li>Place the silico...

<ol>
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Chem. 23 (7), 1640-1648 (2004).</li><li>Vrana, B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Passive+sampling:+An+effective+method+for+monitoring+seasonal+and+spatial+variability+of+dissolved+hydrophobic+organic+contaminants+and+metals+in+the+Danube+river.">Passive sampling: An effective method for monitoring seasonal and spatial variability of dissolved hydrophobic organic contaminants and metals in the Danube river.</a> Environ. Pollut. 184, 101-112 (2014).</li><li>Dougherty, J. A., Swarzenski, P. W., Dinicola, R. 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A. 1218 (51), 9162-9173 (2011).</li><li>Poulier, G., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Estimates+of+pesticide+concentrations+and+fluxes+in+two+rivers+of+an+extensive+French+multi-agricultural+watershed:+application+of+the+passive+sampling+strategy.">Estimates of pesticide concentrations and fluxes in two rivers of an extensive French multi-agricultural watershed: application of the passive sampling strategy.</a> Environ. Sci. Pollut. Res. 22 (11), 8044-8057 (2015).</li><li>Moschet, C., Vermeirssen, E. L. 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Technol. 43 (14), 5383-5390 (2009).</li><li>Vrana, B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Passive+sampling+techniques+for+monitoring+pollutants+in+water.">Passive sampling techniques for monitoring pollutants in water.</a> TrAC - Trend. Anal. Chem. 24 (10), 845-868 (2005).</li><li>Allan, I. J., Harman, C., Ranneklev, S. B., Thomas, K. V., Grung, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Passive+sampling+for+target+and+nontarget+analyses+of+moderately+polar+and+nonpolar+substances+in+water.">Passive sampling for target and nontarget analyses of moderately polar and nonpolar substances in water.</a> Environ. Toxicol. Chem. 32 (8), 1718-1726 (2013).</li><li>Escher, B. I., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Evaluation+of+contaminant+removal+of+reverse+osmosis+and+advanced+oxidation+in+full-scale+operation+by+combining+passive+sampling+with+chemical+analysis+and+bioanalytical+tools.">Evaluation of contaminant removal of reverse osmosis and advanced oxidation in full-scale operation by combining passive sampling with chemical analysis and bioanalytical tools.</a> Environ. Sci. Technol. 45, 5387-5394 (2011).</li><li>Pesce, S., Morin, S., Lissalde, S., Montuelle, B., Mazzella, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Combining+polar+organic+chemical+integrative+samplers+(POCIS)+with+toxicity+testing+to+evaluate+pesticide+mixture+effects+on+natural+phototrophic+biofilms.">Combining polar organic chemical integrative samplers (POCIS) with toxicity testing to evaluate pesticide mixture effects on natural phototrophic biofilms.</a> Environ. Pollut. 159 (3), 735-741 (2011).</li><li>Booij, K., Smedes, F., Van Weerlee, E. M., Honkoop, P. J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Environmental+monitoring+of+hydrophobic+organic+contaminants:+The+case+of+mussels+versus+semipermeable+membrane+devices.">Environmental monitoring of hydrophobic organic contaminants: The case of mussels versus semipermeable membrane devices.</a> Environ. Sci. Technol. 40 (12), 3893-3900 (2006).</li><li>Harman, C., Allan, I. J., Vermeirssen, E. L. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Calibration+and+use+of+the+polar+organic+chemical+integrative+sampler-a+critical+review.">Calibration and use of the polar organic chemical integrative sampler-a critical review.</a> Environ. Toxicol. Chem. 31 (12), 2724-2738 (2012).</li><li>Jonker, M. T. O., Der Heijden, S. A. V. a. n., Kotte, M., Smedes, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Quantifying+the+effects+of+temperature+and+salinity+on+partitioning+of+hydrophobic+organic+chemicals+to+silicone+rubber+passive+samplers.">Quantifying the effects of temperature and salinity on partitioning of hydrophobic organic chemicals to silicone rubber passive samplers.</a> Environ. Sci. Technol. 49 (11), 6791-6799 (2015).</li><li>Jansson, C., Kreuger, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multiresidue+analysis+of+95+pesticides+at+low+nanogram/liter+levels+in+surface+waters+using+online+preconcentration+and+high+performance+liquid+chromatography/tandem+mass+spectrometry.">Multiresidue analysis of 95 pesticides at low nanogram/liter levels in surface waters using online preconcentration and high performance liquid chromatography/tandem mass spectrometry.</a> J. AOAC Int. 93 (6), 1732-1747 (2010).</li><li>Ahrens, L., Daneshvar, A., Lau, A. E., Kreuger, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+five+passive+sampling+devices+for+monitoring+of+pesticides+in+water.">Characterization of five passive sampling devices for monitoring of pesticides in water.</a> J. Chromatogr. A. 1405, 1-11 (2015).</li><li>Royston, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Approximating+the+Shapiro-Wilk+W-test+for+non-normality.">Approximating the Shapiro-Wilk W-test for non-normality.</a> Stat. Comput. 2 (3), 117-119 (1992).</li><li>Gauthier, T. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Detecting+trends+using+Spearman's+rank+correlation+coefficient.">Detecting trends using Spearman's rank correlation coefficient.</a> Environ. Forensics. 2 (4), 359-362 (2001).</li><li>Morin, N., Mi&#232;ge, C., Coquery, M., Randon, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chemical+calibration,+performance,+validation+and+applications+of+the+polar+organic+chemical+integrative+sampler+(POCIS)+in+aquatic+environments.">Chemical calibration, performance, validation and applications of the polar organic chemical integrative sampler (POCIS) in aquatic environments.</a> TrAC - Trend. Anal. Chem. 36, 144-175 (2012).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Water+Quality+-+Sampling+-+Part+23:+Guidance+on+Passive+Sampling+in+Surface+Waters.">Water Quality - Sampling - Part 23: Guidance on Passive Sampling in Surface Waters.</a> ISO 5667-23:2011. , (2011).</li><li>Morin, N., Camilleri, J., Cren-Oliv&#233;, C., Coquery, M., Mi&#232;ge, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Determination+of+uptake+kinetics+and+sampling+rates+for+56+organic+micropollutants+using+"pharmaceutical"+POCIS.">Determination of uptake kinetics and sampling rates for 56 organic micropollutants using "pharmaceutical" POCIS.</a> Talanta. 109, 61-73 (2013).</li></ol>

For quality control, as standard procedure, laboratory blanks, limits of detection (LOD), recoveries, and repeatability were examined23. A few pesticides were detected in the blank samples at low concentration levels. LODs were set as the value of the lowest point on the calibration curve which meets the criteria of a signal to noise ratio of 3. The average LODs were 8.0 pg absolute injected on column for silicone rubber, 1.7 pg absolute for POCIS-A, 1.6 pg absolute for POCIS-B, 3.0 pg absolute for SDB-RPS dis...

Pesticides are continuously introduced to the aquatic environment and may pose a risk to aquatic organisms1. Monitoring of pesticides in the aqueous environment is typically performed using grab sampling, however, this sampling technique does not fully account for temporal variations in concentrations due to fluctuations in flow or episodic inputs (e.g., precipitation, combined sewer overflows, sewage lagoon release)2,3. Thus, monitoring methods need to be improved for a better estimation of environmental risks associated with pesticides. Passive sampling allows continuous monitoring over an extended period of time with minimal infrastructure and low contaminant concentrations4,5.
Passive samplers have been shown to be a valuable tool for the monitoring in groundwater6, fresh water7-10, wastewater11 and marine waters12. Besides monitoring purposes13,14, passive samplers have also been used for non-target analysis15, toxicology testing16,17, and as an alternative to sediment- and biomonitoring18. Passive samplers accumulate chemicals continuously from water and provide time weighted average (TWA) concentrations14. The uptake of the contaminant depends on the sampling rate (RS) and passive sampler-water partition coefficient (KPW), which depends on the passive sampler design, sampler material, physicochemical properties of the contaminant, and environmental conditions (e.g., water turbulence, temperature)13,14,19,20.
The detailed video aims to show how to calibrate and apply passive samplers for pesticides in water. The specific objectives included i) to perform preparation, extraction and instrumental analysis for 124 individual pesticides using five different types of passive samplers, including silicone rubber, polar organic chemical integrative sampler (POCIS)-A, POCIS-B, SDB-RPS and C18 disk, ii) to assess RS and KPW for the pesticides in a laboratory uptake study, and iii) to demonstrate how to select the appropriate passive sampler of the target compound of interest and how to calculate TWA concentrations for the respective passive sampler.
Reference standards and passive sampler devices
Target compounds included 124 legacy and currently used pesticides including herbicides, insecticides and fungicides (Table 1). Internal standard mixture (IS mixture) included fenoprop (2,4,5-TP), clothianidin-D3, ethion and terbuthylazine-D5. Other used chemicals included methanol (MeOH), acetonitrile (ACN), acetone (ACE), dichloromethane (DCM), cyclohexane (CH), ethyl acetate (EA), petroleum ether (PE), 2-propanol, 25% ammonia solution, acetic acid (HAc) and formic acid (FA). Five different passive sampling devices were characterized, including silicone rubber, POCIS-A and POCIS-B, SDB-RPS, and C18 disk1,21.
Table 1. Passive sampler sampling rate (R&#39;S, L day-1), sampler-water partition coefficients (K&#39;PW, L kg-1) and equations (Eq.) used for the calculation of concentrations in field samples for individual pesticidesa. (Reprinted from Journal of Chromatography A, 1405, Lutz Ahrens, Atlasi Daneshvar, Anna E. Lau, Jenny Kreuger, Characterization of five passive sampling devices for monitoring of pesticides in water, 1-11, Copyright (2015), with permission from Elsevier.)22 <a href="https://www.jove.com/files/ftp_upload/54053/Table_1.xlsx" target="_blank">Please click here to download this file.</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>
			<td style="width:164px;">J&#38;W Scientific</td>
			<td style="width:163px;">HP-5MS</td>
			<td>Analytical column for GC-MS</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">Agilent 6460</td>
			<td style="width:164px;">Agilent Technologies</td>
			<td style="width:163px;">6460</td>
			<td>HPLC-MS/MS</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">Strata C18&#8211;E, 20 x 2 mm id and 20&#8211;25 &#956;m particle size</td>
			<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>
		</tr>
		<tr height="21">
			<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>
			<td style="width:163px;">Strata X</td>
			<td style="width:228px;">Online SPE column for LC-MS/MS</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:492px;">Zorbax Eclipse Plus C18</td>
			<td style="width:164px;">Agilent Technologies</td>
			<td style="width:163px;">Zorbax Eclipse Plus C18</td>
			<td>Analytical column for LC-MS/MS</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">Isolute phase separator, 25 mL</td>
			<td style="width:164px;">Biotage</td>
			<td style="width:163px;">120-1907-E</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:492px;">Stainless steel blind rivet, 3.2x10 mm</td>
			<td style="width:164px;">Ejot &#38; Avdel</td>
			<td style="width:163px;">951222</td>
			<td></td>
		</tr>
	</tbody>
</table>

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

Five different water passive samplers were calibrated under laboratory conditions for measurement of 124 legacy and current used pesticides. This study provides a protocol for the passive sampler preparation, calibration, extraction method and instrumental analysis. Sampling rates (RS) and passive sampler-water partition coefficients (KPW) were calculated for silicone rubber, polar organic chemical integrative sampler POCIS-A, POCIS-B, SDB-RPS and C18 disk. The uptake of the selected compounds depended on their physicochemical properties, i.e., silicone rubber showed a better uptake for more hydrophobic compounds (log octanol-water partition coefficient (KOW) &#62; 5.3), whereas POCIS-A, POCIS-B and SDB-RPS disk were more suitable for hydrophilic compounds (log KOW &#60; 0.70).

Five different passive sampler techniques were compared for the uptake of 124 legacy and current used pesticides including silicone rubber (Figure 1), and POCIS A, POCIS B, SDB-RPS and C18 disk (Figure 2). The performance of the extraction method and instrumental analysis was optimized. The outcome of the laboratory uptake experiments can be used to calculate the R&#39;S and log K&#39;PW values (T...

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 (Video) | JoVE 

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

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

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

Research

JoVE Journal

Environment

Waste Water Derived Electroactive Microbial Biofilms: Growth, Maintenance, and Basic Characterization

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The growth of anodic electroactive microbial biofilms from waste water inocula in a fed-batch reactor is demonstrated using a three-electrode setup ...

EPA Method 1615. Measurement of Enterovirus and Norovirus Occurrence in Water by Culture and RT-qPCR. I. Collection of Virus Samples

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Pollutant concentrations and loads in watersheds vary considerably with time and space. Accurate and timely information on the magnitude of pollutants in ...

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Vernal ponds, also referred to as vernal pools, provide critical ecosystem services and habitat for a variety of threatened and endangered species. ...

Experimental Protocol for Detecting Mitochondrial Function in Hepatocytes Exposed to Organochlorine Pesticides

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This paper presents detailed methods on detecting hepatic mitochondrial function for a better understanding the cause of metabolic disorders caused by ...

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Plants possess a powerful system to defend themselves against potential threats by pathogenic fungi. For agriculturally important plants, however, current ...