Name: characterization and application of passive samplers for monitoring of pesticides in water
Uploaded: 2016-08-03T09:00:00.000+00:00
Duration: 10 min 34 s
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。加入50mL EA在提取室和添加250毫升EA和在500毫升圆底烧瓶三种馏程石。 <ol><li>提取室与瓶烧瓶和冷凝器连接。清洗由索氏提取96小时的硅酮橡胶在约80℃，并在温和的氮气随后干燥。 </li></ol></li><li>附加硅橡胶STRI通过包装杆围绕硅橡胶条在保持器（ 图1）PE到不锈钢蜘蛛样品架。硅橡胶带的两端连接到一杆使用电缆扎带持有人。 </li></ol><img alt="图1" src="/files/ftp_upload/54053/54053fig1.jpg" /> 图1.原理硅橡胶。被动采样原理图显示了硅橡胶条纹在不锈钢蜘蛛样品架用从顶部和B）侧视附件）硅橡胶。 <a href="https://www.jove.com/files/ftp_upload/54053/54053fig1large.jpg" target="_blank">请点击此处查看大图这个数字。</a> <ol start="2"><li> POCIS-A和POCIS-B <ol><li>对于POCIS-A，将通过9.0厘米SQUAR 29.0厘米之间220毫克HLB松散的吸着（表面积= 1.78×10 6 平方厘米）的È聚醚砜（PES）膜（ 图2）。 </li><li>对于POCIS-B，放置220毫克的吸附剂混合物的（ 即 ，羟基化的聚苯乙烯-二乙烯基苯树脂（80％）和分散在苯乙烯二乙烯基苯共聚物的碳质吸附剂（20％））（表面积= 2.82×10 6 cm 2）的两者之间的PES膜（ 图2）。 </li><li>压缩吸附剂和手动两个不锈钢环之间有两个PES（内直径= 5.4Hz厘米）和将其固定在不锈钢样品架（ 图2）。 </li></ol></li></ol><img alt="图2" src="/files/ftp_upload/54053/54053fig2.jpg" /> 图2.原理被动采样磁盘。被动采样原理图POCIS A，POCIS B，SDB-RPS盘并呈现出 ）被动取样器的装配采用不锈钢戒指，聚醚砜-C 18盘（PES）MEMBRANES和接收阶段，和B）在不锈钢样品架装配。 <a href="https://www.jove.com/files/ftp_upload/54053/54053fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <ol start="3"><li> SDB-RPS盘和C盘18 <ol><li>放置之间的SDB-RPS（表面积= 35 平方厘米，吸附剂质量= 0.34克，体积= 1.7 毫升 ）和C 18的磁盘（表面积= 35 平方厘米，吸附剂质量= 0.58克，体积= 1.7 毫升 ）两个PE膜（ 图2）。压缩磁盘和手动两个不锈钢环之间有两个PES（内直径= 5.4Hz厘米），将其固定在不锈钢样品架（ 图2）。 </li></ol></li></ol> 2.实验室摄取实验注:进行实验室实验摄取定量表征摄取ķinetics 124个人农药控制的条件下五种不同的被动采样装置。 <ol><li>进行矩形玻璃容器摄取研究（各〜95 L）:坦克1）硅橡胶（N = 16），罐2）POCIS-A（N = 16），POCIS-B（N = 16），和坦克3 ）SDB-RPS盘（N = 16），C 18盘（N = 16）。填写自然水变成了三辆坦克。 </li><li>在恒定水温度（〜20℃），并使用连接于在每一侧的壁两个电动泵湍流水条件（至10厘米秒-1）下进行所有的实验。在黑暗中进行的实验中，以尽量减少光降解​​的效果。 </li><li>穗各玻璃容器与含有用玻璃注射器124杀虫剂杀虫剂标准混合物（三≈400纳克L -1在水箱个别农药）。从储罐手动取出被动采样，在时间间隔5中，11，20，和26ðAYS，确定杀虫剂的采样率。 </li><li>通过在第0天，5，11，20收集100ml水中的样品监测在每个箱中的农药的浓度，和26的水样品的分析如别处21所述进行。 <ol><li>在质量控制方面，在第0天暴露空白样品到室内空气中1小时，然后保存并把它们当作真正的样品。存储所有提取物以及在-18℃直至进一步分析从罐中收集的100ml水中的样品。 </li></ol></li></ol> 3.样品提取<ol><li> 硅橡胶 <ol><li>之前提取，干燥下高纯氮气流的硅橡胶条。 </li><li>气相色谱-质谱（GC-MS）分析，进行使用索氏提取22的固-液萃取。 <ol><li>放置硅橡胶入索氏提取器中。添加250毫升PE / ACE（50/50，体积/体积）和3博伊凌石成圆底烧瓶中。 </li><li>用100μl的尖峰的硅橡胶是用玻璃注射器混合物（C = 5纳克毫升-1）。加入50mL的PE / ACE（50/50，体积/体积）到索氏提取器中。交换机上的加热器和运行索氏提取19小时，然后关闭加热器。 </li><li>通过旋转蒸发然后温和氮气放空到1ml浓缩提取物。通过氮放空到1ml过程中加入三次1毫升CH / ACE（90/10，体积/体积）交换到CH / ACE（90/10，体积/体积）的溶剂。 </li></ol></li><li>用于液相色谱-串联质谱（LC-MS / MS）分析，进行使用索氏提取22的提取。 <ol><li>放置硅橡胶入索氏提取器中。加入250毫升甲醇和3沸腾的石头放入圆底烧瓶和50毫升甲醇成索氏提取器。穗硅橡胶用100μl的IS混合物（C = 5纳克毫升-1）使用玻璃SYR英格。 </li><li>交换机上的加热器和运行索氏提取19小时，然后关闭加热器。通过旋转蒸发然后温和氮气放空到1ml浓缩提取物。通过氮放空至1ml中加入1ml乙腈交换溶剂，乙腈。 </li></ol></li></ol></li><li> POCIS-A和POCIS-B <ol><li>小心地打开POCIS采样，并使用漏斗用超纯水的吸附剂转移到含有两个聚乙烯（PE）玻璃料一个预清洁空聚丙烯固相萃取（SPE）柱（6毫升）中。通过真空干燥吸附剂以除去水。记录空和填充SPE柱的重量来控制吸附剂材料的重量。请注意，不同的墨盒被用于GC-MS和LC-MS / MS分析。 </li><li>之前洗脱，使用玻璃注射器尖峰用100μl的吸附剂IS混合物（C = 5纳克毫升-1）。用5洗脱POCIS-A和POCIS-B吸附剂毫升EA为GC-MS 22。 <ol><li>通过温和氮气放空浓缩萃取液至1ml。通过氮放空到1ml过程中加入三次1毫升CH / ACE（90/10，体积/体积）交换到CH / ACE（90/10，体积/体积）的溶剂。 </li></ol></li><li>用1.5ml的MeOH中，随后用8ml DCM / MeOH中洗脱POCIS-A和POCIS-B柱（80/20，体积/体积）用于LC-MS / MS分析22。通过温和氮气放空浓缩萃取液至1ml。通过氮放空至1ml中加入1ml乙腈交换溶剂，乙腈。 </li></ol></li><li> SDB-RPS和C 18盘 <ol><li>转移SDB-RPS和C 18盘的各个磁盘到一个玻璃烧杯中，并在氮气干燥。用5毫升的EA尖峰用100μl的磁盘IS混合物（C = 5纳克毫升-1）用玻璃注射器和超声处理他们两次在室温下的玻璃烧杯中，首先进行10分钟，然后用3毫升的EA 10分钟。 </li><li>传输博次萃取到一个玻璃管中，将它们集中至2ml通过温和氮气吹下来，然后将它们分成两个1毫升级分（用于GC-MS和LC-MS / MS分析，分别）。 </li><li>通过温和氮气放空浓缩萃取液至0.5 ml和交换溶剂，CH / ACE（90/10，体积/体积）用于GC-MS分析22。通过温和氮气放空浓缩萃取液至0.5 ml和交换溶剂，乙腈用于LC-MS / MS分析22。 </li></ol></li></ol> 4.水样<ol><li>穗用100μl的20毫升水样品IS混合物用玻璃注射器（C = 5纳克毫升-1），加入3毫升DCM中，涡旋3分钟，倾倒到一个相分离器用于GC-MS分析22。 <ol><li>两相分离后，过滤DCM相到玻璃试管中。重复使用3-毫升DCM中的提取，和冲洗用2ml DCM中的管中。最后，通过温和氮气吹下来EXCHAN浓缩萃取液至0.5毫升戈到CH溶剂/ ACE（90/10，体积/体积）。 </li></ol></li><li>分析使用大容量注射剂，类似于通过LC-MS / MS 21别处描述的方法中的水样。 </li></ol> 5.仪器分析<ol><li> GC-MS分析<ol><li>执行使用GC-MS系统，电子电离（EI）和负化学电离（NCI）模式，分别为22的CH / ACE提取物的仪器分析。 </li><li>对于使用EI由GC-MS法，注入1微升用不分流进样方法上的HP-5MS UI柱（30m，0.25内径，0.25微米的膜）等分试样。 </li><li>对于由GC-MS，用方法CI，注入的上一个的HP-5MS UI塔3微升（30米，0.25内径，0.25微米的膜）等分试样。 </li></ol></li><li> HPLC-MS / MS分析<ol><li>执行乙腈的仪器分析提取物用HPLC-MS / MS接口与在负电喷雾电离源（（ - ）。ESI）和正离子米颂（（+）ESI）22。 </li><li>为（+）。ESI，稀释100微升的乙腈用FA调节至pH 5 900微升超纯水提取。 </li><li>对于（ - ）ESI，稀释100微升乙腈的用1％FA的超纯水900微升解提取。 </li><li>为（+）。ESI，使用由2-丙醇/甲醇/ 10mM的甲酸铵（92年6月2日，体积/体积/体积）和MeOH的二元梯度以0.3ml分钟-1的流速。 </li><li>为（ - ）。ESI，使用由乙腈/超纯水0.1％醋酸和ACN + 0.1％醋酸的二元梯度以0.3ml分钟-1的流速。 </li><li>使用的使用两个在线固相萃取柱（均为20×2毫米内径和20至25微米的粒度），以及一个分析柱（C 18，100×3毫米，3.5微米）21 500微升大体积注射注入所有样本。 </li></ol></li></ol> 6.理论的被动采样注:该化学品到被动采样器mediu摄取轮廓米（PSM）被分为三个部分:线性的，曲线的和平衡（ 图3）。 <img alt="图3" src="/files/ftp_upload/54053/54053fig3.jpg" /> 图3.被动采样的吸收曲线。 A）和C）以ng绝对分别脒和乐果，累计量摄取曲线，在被动采样（N t）和B）和D）的脒与乐果，分别以ng升水罐浓度- 1。 <a href="https://www.jove.com/files/ftp_upload/54053/54053fig3large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <ol><li>通过将目标化合物的累积量在被动采样后曝光的吨天（N&#39; 吨计算被动采样器的等效水体积（V 当量 L）的</su通过使用抓斗和时间集成有源采样在水相中的浓度（C W，纳克L-1）P&gt;，纳克）。 <img alt="式（1）" src="/files/ftp_upload/54053/54053eq1.jpg" /> （1） </li><li>派生从摄取轮廓的线性吸收阶段的采样速率（R S，L天-1），通过取V 当量与部署时的斜率。 </li><li>计算在K PW使用公式个别农药（-1大号公斤）。 2。 <img alt="公式（2）" src="/files/ftp_upload/54053/54053eq2.jpg" /> （2） 其中m，p是每采样吸附剂质量（NG）。 </li><li>线性吸收阶段，计算在由被动采样衍生水分析物的TWA浓度（ 三TWA，纳克L-1），使用式3。 <img alt="公式3" src="/files/ftp_upload/54053/54053eq3.jpg" /> （3） 其中R S是SAmpling率（L天-1），t是部署时间（天）。 </li><li>在曲线阶段，用公式计算ÇTWA。 4。 <img alt="公式4" src="/files/ftp_upload/54053/54053eq4.jpg" /> （4） </li><li>在平衡期，用公式计算ÇTWA。 5。 <img alt="公式5" src="/files/ftp_upload/54053/54053eq5.jpg" /> （5） </li></ol> 7.统计数据分析<ol><li>测试使用夏皮罗-威尔克测试23数据的非正态分布。使用在K PW和R S非参数Spearman秩相关VS测试农药的理化性质（斯皮尔曼的Rho范围从-1到1）24。 </li></ol>

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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>

The authors have nothing to disclose.

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><tbody><tr><td>Methanol</td><td>Merck Millipore</td><td>1.06035.2500</td><td></td></tr><tr><td>Acetonitrile</td><td>Merck Millipore</td><td>1.00029.2500&amp;nbsp;</td><td></td></tr><tr><td>Acetone</td><td>Merck Millipore</td><td>1.00012.2500</td><td></td></tr><tr><td>2-propanol</td><td>Merck Millipore</td><td>1.00272.2500</td><td></td></tr><tr><td>Dichloromethane</td><td>Merck Millipore</td><td>1.06054.2500</td><td></td></tr><tr><td>Ammoniak</td><td>Merck Millipore</td><td>1.05428.1000</td><td>Purity 25%</td></tr><tr><td>Formic acid</td><td>Sigma-Aldrich</td><td>94318-50ML-F</td><td>Purity ~98%</td></tr><tr><td>Ethyl acetate&amp;nbsp;</td><td>Sigma-Aldrich</td><td>31063-2.5L</td><td>for pesticide residue analysis</td></tr><tr><td>Petroleum ether&amp;nbsp;</td><td>Sigma-Aldrich</td><td>34491-4X2.5L</td><td>for pesticide residue analysis</td></tr><tr><td>Acetic acid&amp;nbsp;</td><td>Sigma-Aldrich</td><td>320099-500ML</td><td>Purity &amp;ge;99.7%</td></tr><tr><td>Cyclohexane&amp;nbsp;</td><td>Fisher Chemicals</td><td>C/8933/17</td><td>for residue analysis</td></tr><tr><td>Empty polypropylene SPE Tube with PE frits, 20 &amp;mu;m porosity, volume 6&amp;nbsp;ml</td><td>Supelco</td><td>57026</td><td></td></tr><tr><td>Empore SPE Disks, C&lt;sub&gt;18&lt;/sub&gt;, diam. 47&amp;nbsp;mm</td><td>Supelco</td><td>66883-U</td><td>Passive sampler</td></tr><tr><td>Empore SPE Disks, SDB-RPS (Reversed-Phase Sulfonate), diam. 47&amp;nbsp;mm</td><td>Supelco</td><td>66886-U&amp;nbsp;</td><td>Passive sampler</td></tr><tr><td>POCIS-A&amp;nbsp;</td><td>EST</td><td>POCIS-HLB</td><td>Passive sampler</td></tr><tr><td>POCIS-B</td><td>EST</td><td>POCIS-Pesticide&amp;nbsp;</td><td>Passive sampler</td></tr><tr><td>Polyethersulfone (PES) membranes</td><td>EST</td><td>PES</td><td></td></tr><tr><td>Silicone rubber sheet</td><td>Altec</td><td>03-65-4516</td><td>Passive sampler</td></tr><tr><td>Agilent 5975C</td><td>Agilent Technologies</td><td>5975C</td><td>GC-MS</td></tr><tr><td>HP-5MS UI</td><td>J&amp;amp;W Scientific</td><td>HP-5MS</td><td>Analytical column for GC-MS</td></tr><tr><td>Agilent 6460</td><td>Agilent Technologies</td><td>6460</td><td>HPLC-MS/MS</td></tr><tr><td>Strata C18&amp;ndash;E, 20 x 2 mm id and 20&amp;ndash;25 &amp;mu;m particle size</td><td>Phenomenex</td><td>Strata C18&amp;ndash;E</td><td>Online SPE column for LC-MS/MS</td></tr><tr><td>Strata X, 20 x 2 mm id and 20&amp;ndash;25 &amp;mu;m particle size</td><td>Phenomenex</td><td>Strata X</td><td>Online SPE column for LC-MS/MS</td></tr><tr><td>Zorbax Eclipse Plus C18</td><td>Agilent Technologies</td><td>Zorbax Eclipse Plus C18</td><td>Analytical column for LC-MS/MS</td></tr><tr><td>Isolute phase separator, 25 ml</td><td>Biotage</td><td>120-1907-E</td><td></td></tr><tr><td>Stainless steel blind rivet, 3.2x10&amp;nbsp;mm</td><td>Ejot &amp;amp; Avdel</td><td>951222</td><td></td></tr></tbody></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 ...

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Research

JoVE Journal

Environment

9.5K 次观看.  Swedish University of Agricultural Sciences. A protocol about the characterization and application of five different passive sampling devices is presented.

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

Integrated Field Lysimetry and Porewater Sampling for Evaluation of Chemical Mobility in Soils and Established Vegetation

Potentially toxic chemicals are routinely applied to land to meet growing demands on waste management and food production, but the fate of these chemicals is often not well understood. Here we demonstrate an integrated field lysimetry and porewater sampling method for evaluating the mobility of chemicals applied to soils and established vegetation. Lysimeters, open columns made of metal or plastic, are driven into bareground or vegetated soils. Porewater samplers, which are commercially available and use vacuum to collect percolating soil water, are installed at predetermined depths within the lysimeters. At prearranged times following chemical application to experimental plots, porewater is collected, and lysimeters, containing soil and vegetation, are exhumed. By analyzing chemical concentrations in the lysimeter soil, vegetation, and porewater, downward leaching rates, soil retention capacities, and plant uptake for the chemical of interest may be quantified. Because field lysimetry and porewater sampling are conducted under natural environmental conditions and with minimal soil disturbance, derived results project real-case scenarios and provide valuable information for chemical management. As chemicals are increasingly applied to land worldwide, the described techniques may be utilized to determine whether applied chemicals pose adverse effects to human health or the environment.

Field lysimetry and porewater sampling allow researchers to evaluate the fate of chemicals applied to soils and established vegetation. The goal of this protocol is to demonstrate how to install required instrumentation and collect samples for chemical analysis during integrated field lysimetry and porewater sampling experiments.

综合外地Lysimetry和孔隙水采样的化学活动性土壤的评价和植被成立

Potentially toxic chemicals are routinely applied to land to meet growing demands on waste management and food production, but the fate of these chemicals ...

科研

环境科学

Calibrated Passive Sampling - Multi-plot Field Measurements of NH3 Emissions with a Combination of Dynamic Tube Method and Passive Samplers

Agricultural ammonia (NH3) emissions (90% of total EU emissions) are responsible for about 45% airborne eutrophication, 31% soil acidification and 12% fine dust formation within the EU15. But NH3 emissions also mean a considerable loss of nutrients. Many studies on NH3 emission from organic and mineral fertilizer application have been performed in recent decades. Nevertheless, research related to NH3 emissions after application fertilizers is still limited in particular with respect to relationships to emissions, fertilizer type, site conditions and crop growth. Due to the variable response of crops to treatments, effects can only be validated in experimental designs including field replication for statistical testing. The dominating ammonia loss methods yielding quantitative emissions require large field areas, expensive equipment or current supply, which restricts their application in replicated field trials. This protocol describes a new methodology for the measurement of NH3 emissions on many plots linking a simple semi-quantitative measuring method used in all plots, with a quantitative method by simultaneous measurements using both methods on selected plots. As a semi-quantitative measurement method passive samplers are used. The second method is a dynamic chamber method (Dynamic Tube Method) to obtain a transfer quotient, which converts the semi-quantitative losses of the passive sampler to quantitative losses (kg nitrogen ha-1). The principle underlying this approach is that passive samplers placed in a homogeneous experimental field have the same NH3 absorption behavior under identical environmental conditions. Therefore, a transfer co-efficient obtained from single passive samplers can be used to scale the values of all passive samplers used in the same field trial. The method proved valid under a wide range of experimental conditions and is recommended to be used under conditions with bare soil or small canopies (&#60;0.3 m). Results obtained from experiments with taller plants should be treated more carefully.

Calibrated Passive Sampling - Multi-plot Field Measurements of NH3 Emissions with a Combination of Dynamic Tube Method and Passive Samplers

Ammonia emissions are a major threat to the environment by eutrophication, soil acidification and fine particle formation and stem mainly from agricultural sources. This method allows ammonia loss measurements in replicated field trials enabling statistical analysis of emissions and of relationships between crop development and emissions.

校准被动采样 - NH多情节场测量<sub&gt; 3</sub&gt;与动态管法和被动采样的组合排放

Agricultural ammonia (NH3) emissions (90% of total EU emissions) are responsible for about 45% airborne eutrophication, 31% soil acidification and 12% ...

A Simple Method for Automated Solid Phase Extraction of Water Samples for Immunological Analysis of Small Pollutants

A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and enables to perform rapid, automated and simple SPE. The pre-concentrated solution is compatible with analysis by immunoassay, with a low organic solvent content. A method is described for the extraction and pre-concentration of natural hormone 17&#946;-estradiol in 100 ml water samples. Reverse phase SPE is performed with octadecyl-silica sorbent and elution is done with 200 &#181;l of methanol 50% v/v. Eluent is diluted by adding di-water to lower the amount of methanol. After preparing manually the SPE column, the overall procedure is performed automatically within 1 hr. At the end of the process, estradiol concentration is measured by using a commercial enzyme-linked immune-sorbent assay (ELISA). 100-fold pre-concentration is achieved and the methanol content in only 10% v/v. Full recoveries of the molecule are achieved with 1 ng/L spiked de-ionized and synthetic sea water samples.

A protocol for the extraction and pre-concentration of estradiol from water samples by using an automated and miniaturized system is presented.

对水样的自动固相萃取小污染物的免疫学分析的简单方法

A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and ...

Clean Sampling and Analysis of River and Estuarine Waters for Trace Metal Studies

Most of the trace metal concentrations in ambient waters obtained a few decades ago have been considered unreliable owing to the lack of contamination control. Developments of some techniques aiming to reduce trace metal contamination in the last couple of decades have resulted in concentrations reported now being orders of magnitude lower than those in the past. These low concentrations often necessitate preconcentration of water samples prior to instrumental analysis of samples. Since contamination can appear in all phases of trace metal analyses, including sample collection (and during preparation of sampling containers), storage and handling, pretreatments, and instrumental analysis, specific care needs to be taken in order to reduce contamination levels at all steps. The effort to develop and utilize "clean techniques" in trace metal studies allows scientists to investigate trace metal distributions and chemical and biological behavior in greater details. This advancement also provides the required accuracy and precision of trace metal data allowing for environmental conditions to be related to trace metal concentrations in aquatic environments.
This protocol that is presented here details needed materials for sample preparation, sample collection, sample pretreatment including preconcentration, and instrumental analysis. By reducing contamination throughout all phases mentioned above for trace metal analysis, much lower detection limits and thus accuracy can be achieved. The effectiveness of "clean techniques" is further demonstrated using low field blanks and good recoveries for standard reference material. The data quality that can be obtained thus enables the assessment of trace metal distributions and their relationships to environmental parameters.

Special care using "clean techniques" is required to properly collect and process water samples for trace metal studies in aquatic environments. A protocol for sampling, processing, and analytical procedures with the aim of obtaining reliable environmental monitoring data and results with high sensitivity for detailed trace metal studies is presented.

清洁取样和痕量金属研究河和河口水域分析

Most of the trace metal concentrations in ambient waters obtained a few decades ago have been considered unreliable owing to the lack of contamination ...

Protocols for Quantifying Transferable Pesticide Residues in Turfgrass Systems

Plant canopies in established turfgrass systems can intercept an appreciable amount of sprayed pesticides, which can be transferred through various routes onto humans. For this reason, transferable pesticide residue experiments are required for registration and re-registration by the United States Environmental Protection Agency (USEPA). Although such experiments are required, limited specificity is required pertaining to experimental approach. Experimental approaches used to assess pesticide transfer to humans including hand wiping with cotton gloves, modified California roller (moving a roller of known mass over cotton cloth) and soccer ball roll (ball wrapped with sorbent strip) over three treated turfgrass species (creeping bentgrass, hybrid bermudagrass and tall fescue maintained at 0.4, 5 and 9 cm, respectively) are presented. The modified California roller is the most extensively utilized approach to date, and is best suited for use at low mowing heights due to its reproducibility and large sampling area. The soccer ball roll is a less aggressive transfer approach; however, it mimics a very common occurrence in the most popular international sport, and has many implications for nondietary pesticide exposure from hand-to-mouth contact. Additionally, this approach may be adjusted for other athletic activities with limited modification. Hand wiping is the best approach to transfer pesticides at higher mowing heights, as roller-based approaches can lay blades over; however, it is more subjective due to more variable sampling pressure. Utility of these methods across turfgrass species is presented, and additional considerations to conduct transferable pesticide residue research in turfgrass systems are discussed.

Transferable pesticide residue experiments in turfgrass systems are integral components of human risk exposure assessments. Experimental approaches to measure transferable residues should be adjusted to the human interaction of interest and turfgrass system dynamics. Three transferable pesticide residue protocols are presented and the suitability across three turfgrass systems is discussed.

协议在草坪系统量化转换农药残留

Plant canopies in established turfgrass systems can intercept an appreciable amount of sprayed pesticides, which can be transferred through various routes ...

Vegetated Treatment Systems for Removing Contaminants Associated with Surface Water Toxicity in Agriculture and Urban Runoff

Urban stormwater and agriculture irrigation runoff contain a complex mixture of contaminants that are often toxic to adjacent receiving waters. Runoff may be treated with simple systems designed to promote sorption of contaminants to vegetation and soils and promote infiltration. Two example systems are described: a bioswale treatment system for urban stormwater treatment, and a vegetated drainage ditch for treating agriculture irrigation runoff. Both have similar attributes that reduce contaminant loading in runoff: vegetation that results in sorption of the contaminants to the soil and plant surfaces, and water infiltration. These systems may also include the integration of granulated activated carbon as a polishing step to remove residual contaminants. Implementation of these systems in agriculture and urban watersheds requires system monitoring to verify treatment efficacy. This includes chemical monitoring for specific contaminants responsible for toxicity. The current paper emphasizes monitoring of current use pesticides since these are responsible for surface water toxicity to aquatic invertebrates.

This article summarizes the design attributes and the effectiveness of treatment systems that treat urban stormwater and agriculture irrigation runoff to remove pesticides and other contaminants associated with aquatic toxicity.

用于去除与农业和城市径流中地表水毒性有关的污染物的植被处理系统

Urban stormwater and agriculture irrigation runoff contain a complex mixture of contaminants that are often toxic to adjacent receiving waters. Runoff may ...

Continuous Instream Monitoring of Nutrients and Sediment in Agricultural Watersheds

Pollutant concentrations and loads in watersheds vary considerably with time and space. Accurate and timely information on the magnitude of pollutants in water resources is a prerequisite for understanding the drivers of the pollutant loads and for making informed water resource management decisions. The commonly used &#34;grab sampling&#34; method provides the concentrations of pollutants at the time of sampling (i.e., a snapshot concentration) and may under- or overpredict the pollutant concentrations and loads. Continuous monitoring of nutrients and sediment has recently received more attention due to advances in computing, sensing technology, and storage devices. This protocol demonstrates the use of sensors, sondes, and instrumentation to continuously monitor in situ nitrate, ammonium, turbidity, pH, conductivity, temperature, and dissolved oxygen (DO) and to calculate the loads from two streams (ditches) in two agricultural watersheds. With the proper calibration, maintenance, and operation of sensors and sondes, good water quality data can be obtained by overcoming challenging conditions such as fouling and debris buildup. The method can also be used in watersheds of various sizes and characterized by agricultural, forested, and/or urban land.

With the advancement of technology and the rise in end-user expectations, the need and use of higher temporal resolution data for pollutant load estimation has increased. This protocol describes a method for continuous in situ water quality monitoring to obtain higher temporal resolution data for informed water resource management decisions.

农业流域营养盐和泥沙的连续河道监测

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

Capturing Flow-weighted Water and Suspended Particulates from Agricultural Canals During Drainage Events

The purpose of this study is to describe the methods used to capture flow-weighted water and suspended particulates from farm canals during drainage discharge events. Farm canals can be enriched by nutrients such as phosphorus (P) that are susceptible to transport. Phosphorus in the form of suspended particulates can significantly contribute to the overall P loads in drainage water. A settling tank experiment was conducted to capture suspended particulates during discrete drainage events. Farm canal discharge water was collected in a series of two 200 L settling tanks over the entire duration of the drainage event, so as to represent a composite subsample of the water being discharged. Imhoff settling cones are ultimately used to settle out the suspended particulates. This is achieved by siphoning water from the settling tanks via the cones. The particulates are then collected for physico-chemical analyses.

Nutrients present in particulate form can contribute significantly to the overall loads in agricultural drainage waters. This study describes a novel method to capture flow-weighted water and suspended particulates from farm canal drainage over the entire duration of the drainage event.

在排水过程中捕获农用运河中的流动加权水和悬浮颗粒

The purpose of this study is to describe the methods used to capture flow-weighted water and suspended particulates from farm canals during drainage ...

Continuous Hydrologic and Water Quality Monitoring of Vernal Ponds

Vernal ponds, also referred to as vernal pools, provide critical ecosystem services and habitat for a variety of threatened and endangered species. However, they are vulnerable parts of the landscapes that are often poorly understood and understudied. Land use and management practices, as well as climate change are thought to be a contribution to the global amphibian decline. However, more research is needed to understand the extent of these impacts. Here, we present methodology for characterizing a vernal pond's morphology and detail a monitoring station that can be used to collect water quantity and quality data over the duration of a vernal pond's hydroperiod. We provide methodology for how to conduct field surveys to characterize the morphology and develop stage-storage curves for a vernal pond. Additionally, we provide methodology for monitoring the water level, temperature, pH, oxidation-reduction potential, dissolved oxygen, and electrical conductivity of water in a vernal pond, as well as monitoring rainfall data. This information can be used to better quantify the ecosystem services that vernal ponds provide and the impacts of anthropogenic activities on their ability to provide these services.

Understanding the ecosystem services and processes provided by vernal ponds and the impacts of anthropogenic activities on their ability to provide these services requires intensive hydrologic monitoring. This sampling protocol using in-situ monitoring equipment was developed to understand the impact of anthropogenic activities on water levels and quality.

春季池塘连续水文水质监测

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

Identifying Per- and Polyfluorinated Chemical Species with a Combined Targeted and Non-Targeted-Screening High-Resolution Mass Spectrometry Workflow

Historical and emerging per- and polyfluoroalkyl substances (PFASs) have garnered significant interest from the public and government agencies from the local to federal levels. The continuing evolution of PFAS chemistries presents a challenge to the environmental monitoring, where ongoing development of targeted methods necessarily lags the discovery of new chemical compounds. There is a need, therefore, to have forward-looking methodologies that can detect emerging and unexpected compounds, monitor these species over time, and resolve details of their chemical structure to enable future work in human health. To this end, non-targeted analysis by high-resolution mass spectrometry offers a broad base detection approach that can be combined with almost any sample preparation scheme and provides significant capabilities for compound identification after detection. Herein, we describe a solid-phase extraction (SPE) based sample concentration method tuned for shorter chain and more hydrophilic PFAS chemistries, such as per fluorinated ether acids and sulfonates, and describe analysis of samples prepared in this fashion in both targeted and non-targeted modes. Targeted methods provide superior quantification when reference standards are available but are intrinsically limited to expected compounds when performing analysis. In contrast, a non-targeted approach can identify the presence of unexpected compounds and provide some information about their chemical structure. Information about chemical features can be used to correlate compounds across sample locations and track abundance and occurrence over time.

Here, we present a protocol for the sequential targeted quantification and non-targeted analysis of fluorinated compounds in water by mass spectrometry. This methodology provides quantitative levels of known fluorochemical compounds and identifies unknown chemicals in related samples with semi-quantitative estimates of their abundance.

利用目标筛选和非靶向筛选高分辨率质谱相结合的工作流程识别跨氟和多氟化学物种

Historical and emerging per- and polyfluoroalkyl substances (PFASs) have garnered significant interest from the public and government agencies from the ...