Name: extraction of organochlorine pesticides from plastic pellets and plastic type analysis
Uploaded: 2017-07-01T13:00:00.000+00:00
Duration: 10 min 12 s
Description: Watch this Scientific Journal Video about Extraction of Organochlorine Pesticides from Plastic Pellets and Plastic Type Analysis at JoVE.com

这项工作由DeFishGear项目（1°str / 00010）内的"2007 - 2013年IPA亚得里亚尔跨境合作计划"资助。

塑料颗粒取样<ol><li>在进入现场之前，用丙酮或乙醇（99％）三次冲洗所有必需的采样材料（ 如镊子和铝箔）。在材料不能进行溶剂冲洗的情况下，在烘箱（ 例如玻璃器皿）中将其在450℃下加热过夜。 注意:在旅游区域，请获取有关清除大部分海洋垃圾（包括微量塑料）的海滩清洁活动的信息。如果可能，在此操作之前规划采样。如果在清理季节进行抽样，请以身份证明文件（ 例如，日期，清理方法等 ）指定此活动的详细信息。 </li><li>穿戴手套，用溶剂冲洗的不锈钢镊子从海滩收集塑料颗粒。 </li><li>每个位置样品50至100个颗粒，其对应于每个位置5至10个重复（每个重复10个颗粒）。如果所需的颗粒数不能达到收集最大的粒子可能，并在身份海滩表格中指定。 </li><li>在采样结束时，将收集的颗粒包裹在溶剂冲洗的铝箔中。玻璃瓶可以用作替代甚至纸袋。 </li><li>填写所选海滩的身份证件，其中包含缺少的信息（ 即海滩位置，天气状况，细粒度等 ）。 </li><li>如果环境温度超过25°C，将样品运送到实验室。在短途旅行的情况下可以跳过此步骤（ 例如 &lt;1 h）。 </li><li>一旦在实验室中，轻轻擦拭颗粒中的可移除颗粒（ 例如沙子）。在干燥器中，必要时将样品干燥，然后储存（黑暗，T &lt;25°C）。避免可能使用OCP的房间（ 例如，存储标准解决方案）。 </li><li>短时间内（ 即几天）将冰球储存在冰箱中（4℃）在冷冻器（-18°C）下，在溶剂冲洗的铝箔中更长时间。 </li><li>避免将样品暴露在人造光线或阳光下。在分析前尽可能少地处理样品以降低污染风险。 </li></ol> 2.从塑料颗粒中提取OCP <ol><li>为了减少污染的风险，请在干净的实验室中使用经过仔细洗涤的玻璃器皿进行如下操作:2次用分析纯丙酮，二氯甲烷和正己烷冲洗。在氮气流下干燥玻璃器皿，防止与环境空气接触（ 例如，带有清洁铝箔的盖子）。在协议的进一步步骤（ 即第3节和第4节）中应用此清洗程序。 </li><li>使用溶剂冲洗镊子，按以下类别的颜色对颗粒进行分类:白色/透明，白色/淡黄色，黄色/橙色，琥珀色/棕色和着色（ 例如红，绿，蓝等 ） </li><li>收集10粒随机（ 即不考虑塑料类型）的相似颜色，将构成一个复制。 </li><li>称量样品在分析天平上并记录质量。在这个阶段，样品可放回冰箱或冰柜。 </li><li>要考虑到背景污染，请使用每组重复进行空白样品（ 例如， 5个重复的1个空白）。为此，应用与上述相同的方案，但不要在提取池中加入塑料颗粒。该空白样品将经历该方案的进一步步骤，并与样品一起分析。 </li><li> 打开PFE。下载提取方法并将仪器预热至60°C。方法的细节如下: <ol><li>将温度设置为60°C，压力设置为100 bar。 </li><li>选择一个循环，加热时间为1分钟，保持时间为25分钟，放电时间为2分钟。 </li><li>设置溶剂和气体（​​N 2 ）冲洗次数，每次3分钟。 </li><li>选择正己烷作为提取溶剂。 </li></ol></li><li> 仪器升温时，如下所述准备萃取池。如有必要，请将协议修改为供应商仪器说明: <ol><li>将底部过滤器和玻璃料放在提取池中。关闭它并关闭它。 </li><li>使用漏斗用清洁的石英砂填充约一半的电池。 </li><li>加入称重的样品（ 即 10个颗粒的一个重复物）。冷冻塑料颗粒应在提取前放置在冰箱过夜。 </li><li>从细胞顶部加1厘米的石英砂。特别注意使用超清洁石英砂（或玻璃珠），因为它暴露在与样品相同的提取条件下。为了清洁沙子，在分析纯二氯甲烷和正己烷中依次将其萃取到PFE中，加入2或每个溶剂更多的循环（ 例如，在100℃下在100巴下30分钟）。或者，使用超声波浴和/或旋转蒸发器。必要时重复清洁程序。 </li><li>将顶部过滤器插入单元格中，并将单元格放在仪器中。 </li></ol></li><li>将收集容器放入仪器中，开始萃取方法（总运行约35分钟）。 </li><li>当方法完成后，将清洗的玻璃容器（ 例如烧杯，玻璃细胞培养皿）中的提取细胞清空，并在砂中取回10个丸粒。将其储存在容器中，直到进一步分析塑料鉴定（ 如拉链袋或玻璃瓶）。 </li></ol> 3.提取物的浓缩和清除<ol><li>将获得的提取物（约40mL）从收集容器转移到玻璃管中，并在设定为35℃的旋转浓缩器中蒸发至1mL 20分钟。可以使用替代方法ch在氮气流或蒸发器下蒸发。温度和持续时间应相应优化。 </li><li> 同时，通过将废物管放置在机架中，并在紧闭阀位置的歧管上装满活化硅酸镁吸附剂（1g）的填料，准备固相萃取器（SPE）。清理方法基于EPA方法3620C 22 ，如下所示: <ol><li>在源处打开真空，并在筒中加入4 mL己烷以活化吸附剂。 </li><li>打开阀门，让溶剂通过整个吸附剂床。然后关闭阀门，让吸附剂在己烷中浸泡5分钟。 </li><li>打开阀门，使溶剂通过，但在吸附剂干燥之前关闭阀门。 </li><li>当样品浓缩时，用玻璃巴斯德吸管将其转移到药筒。轻轻打开阀门，让其缓慢通过。每秒1-2滴一个适当的速度。 </li><li>用0.5 mL己烷冲洗含有提取物的玻璃管，当提取物通过时将其加入到药筒中。 </li><li>当整个溶剂通过时，关闭阀门并关闭真空。 </li><li>用收集管更换废液管，并使用干净的溶剂导向针。 </li><li>将9mL丙酮/己烷（10/90，v / v）加入到筒中，并在源处打开真空。使吸附剂在溶剂中浸泡1分钟。 </li><li>打开阀门并收集收集管中的整个洗脱液。 </li></ol></li><li>将收集管置于浓缩器中，在35℃下蒸发溶剂9分钟，以达到1 mL洗脱液。 </li><li>将浓缩的洗脱液转移到带有玻璃巴斯德吸管的琥珀自动进样器小瓶中。在这个阶段，样品可以在分析前储存在冰箱中。 </li></ol> 4.清洁和集中的分析提取物<ol><li> 下载GC-μECD仪器（装有微电子捕获检测器的气相色谱仪）控制软件的分析方法。方法的细节如下: <ol><li>将进样器设置为不分流模式，将其温度设置为250°C，将吹扫时间设置为1分钟。 </li><li>将载气（He）的流量设定为1.5 mL / min。 </li><li>对柱式炉进行以下温度梯度的校准:60°C保持1分钟，斜坡为30°C min -1至200°C，斜坡为5°C min -1至230°C，坡度为3°C -1达到250℃，保持该温度5分钟。 </li><li>将检测器温度设置为300℃，备用气体流量（N 2 ）设定为60 mL / min。 </li></ol></li><li>将含有样品的小瓶（清洁并浓缩）放入自动进样器架中，运行方法（运行时间为23.3分钟）。一世<html> nject 2μL样品。 </li><li>分析后，通过其保留时间确定色谱图上的不同化合物，并记录相应的峰面积。 </li><li>考虑到回收率（R）和峰面积（A 1 ），使用校准曲线的方程式计算提取物中每个OCP的浓度（C 1 ）如下: <img alt="公式1" src="/files/ftp_upload/55531/55531eq1.jpg" /> 其中b是原点的截距， a是校准方程的斜率， <img alt="方程式2" src="/files/ftp_upload/55531/55531eq2.jpg" /></li><li>考虑到复制物的质量（m）（ 即 10粒，参见2.4）和最终提取物的体积（V）（ 即 1 mL），计算吸附在每个OCP上的每个OCP的浓度（C 2 ）塑料颗粒（ 即每克塑料颗粒的OCP ng）: /ftp_upload/55531/55531eq3.jpg"/&gt; </li></ol> 5.塑料类型识别<ol><li>将颗粒转移到玻璃培养皿中并将其放在塑料袋中。 </li><li>用镊子握住一个颗粒，并用手术刀切片。塑料袋防止在切割过程中颗粒的损失。 </li><li>用乙醇清洗FT-IR仪器的衰减全反射（ATR）晶体。 </li><li>记录背景光谱。 </li><li>将碎片放在ATR晶体上，并拧紧样品架。该片的内侧必须与晶体接触。 </li><li>扫描样品并记录光谱。 </li><li>通过将获得的光谱与光谱库比较来鉴定构成塑料颗粒的聚合物。虽然更耗时，但是所获得的光谱的解释也可以手动进行，但很可能没有达到图书馆海实现的特异度RCH。 </li></ol>

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<html>大多数关注与塑料颗粒相关的有机污染物的研究依赖于吸附化学品的经典萃取方法。索格利特设备是使用最广泛的技术，典型的萃取时间为12至24小时，有机溶剂的消耗量较高（ 即每次萃取为100至250 mL）。浸渍提取需要样品和有机溶剂之间的长时间接触（ 例如 6天） 4，并可以通过加入超声波步骤来加速。相比之下，如本研究中所述，加压流体萃取是使用减少量...

塑料的全球生产自1950年代以来不断上升，2014年达到3.11亿吨，包装用量约为40％ 1 。同时，越来越多的这些材料正在积累在环境中，这可能对生态系统构成严重威胁2 。尽管在七十年代已经报道，过去十年来，海洋环境中塑料碎屑的发生受到更多的关注。特别是微塑料，直径≤5毫米的塑料碎片现在被认为是主要的海洋水质问题之一3 。 塑料树脂颗粒是通常为圆柱形或圆盘形并且直径为几毫米（ 例如 2至5毫米） 4,5的小颗粒。它们属于微塑料类。这些塑料颗粒是通过在高温下再熔化和成型制造最终塑料制品的工业原料6 。在制造和运输过程中，它们可能会无意中释放到环境中。例如，他们可以在航运4,7,8期间通过意外泄漏直接引入海洋。它们可以通过地表径流，溪流和河流从陆地运送到海洋。由于环保持续，塑料颗粒广泛分布在海洋中，在世界各地的海滩上发现4 。它们可以对海洋生物产生负面影响，并可进入食物链，其影响是不可预知的。此外，一些研究已经揭示了吸附在海岸收集的塑料颗粒上的环境污染物的存在l环境，作为这些潜在有毒化学物质的载体4,9,10。事实上，有实验室证据表明，这些化学物质在从摄入的塑料碎片11,12中释放后，可以在生物体的组织中生物累积。 为了更好地评估与海洋环境中塑料颗粒发生相关的危害，有必要开发可以确定吸附的有机污染物的方法。一个重要的步骤是从塑料基质中提取化学物质，这取决于聚合物类型，其降解阶段和预处理，它们可以呈现异质的物理化学特性。文献中大多数调查报告使用浸渍或索氏提取技术4 ，5，6，9，13，14，15，16，17，18 ，它们是溶剂和/或耗时的。关于这个问题日益增长的兴趣，应该开发替代品，以便更快速地评估吸附在塑料件上的有机污染物。此外，塑料化学分析提供有关微塑料化学结构的信息。结果，可以评估存在于环境中的主要类型的聚合物和共聚物。虽然塑料碎片通常由聚乙烯（PE）和聚丙烯（PP） 5制成，但是一些采样位置可以呈现出其他类别被显着表示的特定轮廓（ 例如，乙烯/乙酸乙烯酯共聚物和聚苯乙烯（PS））。 FT-IR光谱学是一种可靠和用户友好的聚合物识别技术，通常用于识别微塑料19,20 。 本工作的主要目的是提供一种通过PFE从塑料颗粒中提取OCP和相关化合物的快速简便方案。然而，方案的设计包括导致吸附的OCP的确定的所有步骤，从树脂颗粒的取样到化合物的分析。还描述了识别塑料类型的方法。开发的方法论重点是11种OCPs和相关化合物:i）DDT（2,4&#39;-和4,4&#39;-二氯二苯基三氯乙烷）及其两种主要代谢物DDE（2,4&#39;-和4,4&#39;-二氯二苯基二氯乙烯）和DDD （2,4&#39;-和4,4&#39;-二氯二苯基二氯乙烷）; ii）异构体γ-六氯环己烷（γ-HCH）为主要成分农药林丹和生产过程中释放的两种异构体α-HCH和β-HCH 15 ; iii）和技术硫丹中存在的两种生物活性异构体硫丹I（Endo I）和II（Endo II）。所研究的农药是"斯德哥尔摩公约" 21所规定的广谱杀虫剂，化学稳定，疏水性和分类为持久性有机污染物质。

<table><tbody><tr><td>Alpha&amp;ndash;HCH</td><td>Dr. Ehrenstorfer, Augsburg, Germany</td><td>DRE-C14071000</td><td>H301, H351, H400, H410, H312</td></tr><tr><td>Beta&amp;ndash;HCH</td><td>Fluka, Sigma-Aldrich, St. Louis, USA</td><td>33376-100MG</td><td>H301, H312, H351, H410</td></tr><tr><td>Lindane</td><td>Fluka, Sigma-Aldrich, St. Louis, USA</td><td>45548-250MG</td><td>H301, H312, H332, H362, H410</td></tr><tr><td>Endosufan I</td><td>Supleco, Sigma-Aldrich Bellefonte, PA, USA</td><td>48576-25MG</td><td>H301, H410</td></tr><tr><td>Endosulfan II</td><td>Supleco, Sigma-Aldrich, Bellefonte, PA, USA</td><td>48578-25MG</td><td>H301, H410</td></tr><tr><td>2,4&#039;&amp;ndash;DDD</td><td>Fluka, Sigma-Aldrich, St. Louis, USA</td><td>35485-250MG</td><td>H351</td></tr><tr><td>4,4&amp;rsquo;&amp;ndash;DDD</td><td>Dr. Ehrenstorfer, Augsburg, Germany</td><td>DRE-C12031000</td><td>H301, H351, H400, H410, H312</td></tr><tr><td>2,4&amp;rsquo;&amp;ndash;DDE</td><td>Dr. Ehrenstorfer, Augsburg, Germany</td><td>DRE-C12040000</td><td>H351, H400, H410, H302</td></tr><tr><td>4,4&amp;rsquo;-DDE</td><td>Fluka , Sigma-Aldrich, St. Louis, USA</td><td>35487-250MG</td><td>H302, H351, H410</td></tr><tr><td>2,4&amp;rsquo;&amp;ndash;DDT</td><td>Dr. Ehrenstorfer, Augsburg, Germany</td><td>DRE-C12081000</td><td>H301, H311, H330, H351, H400, H410</td></tr><tr><td>4,4&amp;rsquo;&amp;ndash;DDT</td><td>National Institute of Standards and Technology, Gaithersburg, USA</td><td>RM8469-4,4&#039;-DDT</td><td>H301, H311, H351, H372, H410</td></tr><tr><td>n-Hexane&amp;nbsp;</td><td>VWR International GmbH, Graumanngasse, Viena, Austria</td><td>83992.320</td><td>H225, H315, H336, H373, H304, H411</td></tr><tr><td>Acetone for HPLC</td><td>J.T.Baker, Avantor performance Materials B.V., Teugseweg, Netherlands</td><td>8142</td><td>H225, H319, H 336</td></tr><tr><td>FL-PR Florisil 1000mg/6mL</td><td>Phenomenex, Torrance, CA, USA</td><td>8B-S013-JCH</td><td></td></tr><tr><td>Fat free quartz sand 0.3-0.9 mm</td><td>Buchi, Flawil, Switzerland</td><td>37689</td><td></td></tr><tr><td>Gas chromatograph Hawlett Packard HP 6890 Series gas chromatograph with GERSTEL MultiPurpose Sampler MPS 2XL with ECD and FID detector</td><td>Agilent technologies, Santa Clara USA</td><td></td><td></td></tr><tr><td>Presure fluid extractor, Speed Extractor E-916</td><td>Buchi, Flawil, Switzerland</td><td></td><td></td></tr><tr><td>Solid phase extractor</td><td>Supleco, Sigma-Aldrich Bellefonte, PA, USA</td><td></td><td></td></tr><tr><td>Concentrator miVac DUO</td><td>Genevac SP Scientific, Suffolk UK</td><td></td><td></td></tr><tr><td>GC capillary column Zebron ZB-XLB (30 x 0.25 x 0.25)</td><td>Phenomenex, Torrance, CA, USA</td><td>122-1232</td><td></td></tr><tr><td>ATR FT-IR Spectrometer, Spectrum-Two</td><td>Perkin Elmer</td><td></td><td></td></tr></tbody></table>

extraction of organochlorine pesticides from plastic pellets and plastic type analysis

分类为微塑料（直径≤5mm）的塑料树脂颗粒是在制造和运输过程中可能无意中释放到环境中的小颗粒。由于环境的持续存在，广泛分布于世界各地的海洋和海滩。它们可以作为潜在有毒有机化合物（ 例如多氯联苯）的载体，因此可能 对海洋生物有不利影响。它们对食物链的可能影响尚未明了。为了评估与海洋环境中塑料颗粒发生相关的危害，有必要开发允许快速测定相关有机污染物水平的方法。本协议描述了采样树脂颗粒，分析吸附的有机氯农药（OCPs）和识别塑料类型所需的不同步骤。重点是通过加压流体萃取器（PFE）和使用傅立叶变换红外（FT-IR）光谱的聚合物化学分析从塑料颗粒中提取OCP。开发的方法论重点关注11种OCP和相关化合物，包括二氯二苯基三氯乙烷（DDT）及其两种主要代谢产物，林丹和两种生产异构体，以及技术硫丹的两种生物活性异构体。该方案构成了用于评估吸附在塑料片上的有机污染物浓度的现有方法的简单而快速的替代方法。

通常沿着沙滩的高潮和低潮线发现塑料颗粒（ 图1A ）。他们也可以在暴风雨之后坚持海藻新鲜搁浅的海草。它们偶尔会被发现在堆积区域的卵石和石块海滩。 塑料颗粒通常可以通过其形状，尺寸和颜色容易地识别， 如图1B所示（参见两个中间柱）。它们可能被误认为微小的碎石（?...

Watch this Scientific Journal Video about Extraction of Organochlorine Pesticides from Plastic Pellets and Plastic Type Analysis at JoVE.com

Extraction of Organochlorine Pesticides from Plastic Pellets and Plastic Type Analysis

微量塑料作为潜在有毒有机污染物的载体，具有不可预知的作用。该方案描述了一种评估吸附在塑料颗粒上的有机氯农药水平的替代方法，并确定了聚合物的化学结构。重点是加压流体萃取和衰减全反射傅立叶变换红外光谱。

从塑料颗粒中提取有机氯农药和塑料类型分析

Plastic resin pellets, categorized as microplastics (&#8804;5 mm in diameter), are small granules that can be unintentionally released to the environment ...

extraction-organochlorine-pesticides-from-plastic-pellets-plastic

Research

JoVE Journal

Environment

11.5K 次观看.  University of Nova Gorica. 微量塑料作为潜在有毒有机污染物的载体，具有不可预知的作用。该方案描述了一种评估吸附在塑料颗粒上的有机氯农药水平的替代方法，并确定了聚合物的化学结构。重点是加压流体萃取和衰减全反射傅立叶变换红外光谱。 

视频: Extraction of Organochlorine Pesticides from Plastic Pellets and Plastic Type Analysis

Laboratory Estimation of Net Trophic Transfer Efficiencies of PCB Congeners to Lake Trout (Salvelinus namaycush) from Its Prey

A technique for laboratory estimation of net trophic transfer efficiency (&#947;) of polychlorinated biphenyl (PCB) congeners to piscivorous fish from their prey is described herein. During a 135-day laboratory experiment, we fed bloater (Coregonus hoyi) that had been caught in Lake Michigan to lake trout (Salvelinus namaycush) kept in eight laboratory tanks. Bloater is a natural prey for lake trout. In four of the tanks, a relatively high flow rate was used to ensure relatively high activity by the lake trout, whereas a low flow rate was used in the other four tanks, allowing for low lake trout activity. On a tank-by-tank basis, the amount of food eaten by the lake trout on each day of the experiment was recorded. Each lake trout was weighed at the start and end of the experiment. Four to nine lake trout from each of the eight tanks were sacrificed at the start of the experiment, and all 10 lake trout remaining in each of the tanks were euthanized at the end of the experiment. We determined concentrations of 75 PCB congeners in the lake trout at the start of the experiment, in the lake trout at the end of the experiment, and in bloaters fed to the lake trout during the experiment. Based on these measurements, &#947; was calculated for each of 75 PCB congeners in each of the eight tanks. Mean &#947; was calculated for each of the 75 PCB congeners for both active and inactive lake trout. Because the experiment was replicated in eight tanks, the standard error about mean &#947; could be estimated. Results from this type of experiment are useful in risk assessment models to predict future risk to humans and wildlife eating contaminated fish under various scenarios of environmental contamination.

Laboratory Estimation of Net Trophic Transfer Efficiencies of PCB Congeners to Lake Trout Salvelinus namaycush from Its Prey

A technique for laboratory estimation of net trophic transfer efficiency of polychlorinated biphenyl (PCB) congeners to piscivorous fish from their prey is presented. To maximize applicability of the laboratory results to the field, the piscivorous fish should be fed prey fish that are typically eaten in the field.

多氯联苯同系物净营养转移效率湖鳟鱼实验室估计（<em&gt;红点鲑namaycush</em&gt;），从它的猎物

A technique for laboratory estimation of net trophic transfer efficiency (&#947;) of polychlorinated biphenyl (PCB) congeners to piscivorous fish from ...

科研

环境科学

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).

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 ...

Protocol for Microplastics Sampling on the Sea Surface and Sample Analysis

Microplastic pollution in the marine environment is a scientific topic that has received increasing attention over the last decade. The majority of scientific publications address microplastic pollution of the sea surface. The protocol below describes the methodology for sampling, sample preparation, separation and chemical identification of microplastic particles. A manta net fixed on an &#187;A frame&#171; attached to the side of the vessel was used for sampling. Microplastic particles caught in the cod end of the net were separated from samples by visual identification and use of stereomicroscopes. Particles were analyzed for their size using an image analysis program and for their chemical structure using ATR-FTIR and micro FTIR spectroscopy. The described protocol is in line with recommendations for microplastics monitoring published by the Marine Strategy Framework Directive (MSFD) Technical Subgroup on Marine Litter. This written protocol with video guide will support the work of researchers that deal with microplastics monitoring all over the world.

The protocol below describes the methodology for: microplastics sampling on the sea surface, separation of microplastic and chemical identification of particles. This protocol is in line with the recommendations for microplastics monitoring published by the MSFD Technical Subgroup on Marine Litter.

协议塑料微粒采样的海面和样品分析

Microplastic pollution in the marine environment is a scientific topic that has received increasing attention over the last decade. The majority of ...

An Ultra-clean Multilayer Apparatus for Collecting Size Fractionated Marine Plankton and Suspended Particles

The distributions of many trace elements in the ocean are strongly associated with the growth, death, and re-mineralization of marine plankton and those of suspended/sinking particles. Here, we present an all plastic (Polypropylene and Polycarbonate), multi-layer filtration system for collection of suspended particulate matter (SPM) at sea. This ultra-clean sampling device has been designed and developed specifically for trace element studies. Meticulous selection of all non-metallic materials and utilization of an in-line flow-through procedure minimizes any possible metal contamination during sampling. This system has been successfully tested and tweaked for determining trace metals (e.g., Fe, Al, Mn, Cd, Cu, Ni) on particles of varying size in coastal and open ocean waters. Results from the South China Sea at the South East Asia Time-Series (SEATS) station indicate that diurnal variations and spatial distribution of plankton in the euphotic zone can be easily resolved and recognized. Chemical analysis of size-fractionated particles in surface waters of the Taiwan Strait suggests that the larger particles (&#62;153 &#181;m) were mostly biologically derived, while the smaller particles (10 - 63 &#181;m) were mostly composed of inorganic matter. Apart from Cd, the concentrations of metals (Fe, Al, Mn, Cu, Ni) decreased with increasing size.

Plankton and suspended particles play a major role in the biogeochemical cycles in the ocean. Here, we provide an ultra-clean, low stress method for the collection of various sizes of particles and plankton at sea with the capability of handling large volumes of seawater.

海洋浮游生物和悬浮颗粒的超洁净多层采集装置

The distributions of many trace elements in the ocean are strongly associated with the growth, death, and re-mineralization of marine plankton and those ...

Sampling, Sorting, and Characterizing Microplastics in Aquatic Environments with High Suspended Sediment Loads and Large Floating Debris

The ubiquitous presence of plastic debris in the ocean is widely recognized by the public, scientific communities, and government agencies. However, only recently have microplastics in freshwater systems, such as rivers and lakes, been quantified. Microplastic sampling at the surface usually consists of deploying drift nets behind either a stationary or moving boat, which limits the sampling to environments with low levels of suspended sediments and floating or submerged debris. Previous studies that employed drift nets to collect microplastic debris typically used nets with &#8805;300 &#181;m mesh size, allowing plastic debris (particles and fibers) below this size to pass through the net and elude quantification. The protocol detailed here enables: 1) sample collection in environments with high suspended loads and floating or submerged debris and 2) the capture and quantification of microplastic particles and fibers &lt;300 &#181;m. Water samples were collected using a peristaltic pump in low-density polyethylene (PE) containers to be stored before filtering and analysis in the lab. Filtration was done with a custom-made microplastic filtration device containing detachable union joints that housed nylon mesh sieves and mixed cellulose ester membrane filters. Mesh sieves and membrane filters were examined with a stereomicroscope to quantify and separate microplastic particulates and fibers. These materials were then examined using a micro-attenuated total reflectance Fourier transform infrared spectrometer (micro ATR-FTIR) to determine microplastic polymer type. Recovery was measured by spiking samples using blue PE particulates and green nylon fibers; percent recovery was determined to be 100% for particulates and 92% for fibers. This protocol will guide similar studies on microplastics in high velocity rivers with high concentrations of sediment. With simple modifications to the peristaltic pump and filtration device, users can collect and analyze various sample volumes and particulate sizes.

Most microplastic research to date has occurred in marine systems where suspended solid levels are relatively low. Focus is now shifting to freshwater systems, which may feature high sediment loads and floating debris. This protocol addresses collecting and analyzing microplastic samples from aquatic environments that contain high suspended solid loads.

高悬浮泥沙荷载和大型漂浮碎屑水生环境中 Microplastics 的取样、分类和表征

The ubiquitous presence of plastic debris in the ocean is widely recognized by the public, scientific communities, and government agencies. However, only ...

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 ...

Sampling, Identification and Characterization of Microplastics Release from Polypropylene Baby Feeding Bottle during Daily Use

Microplastics (MPs) are becoming a global concern due to the potential risk to human health. Case studies of plastic products (i.e., plastic single-use cups and kettles) indicate that MP release during daily use can be extremely high. Precisely determining the MP release level is a crucial step to identify and quantify the exposure source and assess/control the corresponding risks stemming from this exposure. Though protocols for measuring MP levels in marine or freshwater has been well developed, the conditions experienced by household plastic products can vary widely. Many plastic products are exposed to frequent high temperatures (up to 100 &#176;C) and are cooled back to room temperature during daily use. It is therefore crucial to develop a sampling protocol that mimics the actual daily-use scenario for each particular product. This study focused on widely used polypropylene-based baby feeding bottles to develop a cost-effective protocol for MP release studies of many plastic products. The protocol developed here enables: 1) prevention of the potential contamination during sampling and detection; 2) realistic implementation of daily-use scenarios and accurate collection of the MPs released from baby feeding bottles based on WHO guidelines; and 3) cost-effective chemical determination and physical topography mapping of MPs released from baby feeding bottles. Based on this protocol, the recovery percentage using standard polystyrene MP (diameter of 2 &#181;m) was 92.4-101.2% while the detected size was around 102.2% of the designed size. The protocol detailed here provides a reliable and cost-effective method for MP sample preparation and detection, which can substantially benefit future studies of MP release from plastic products.

This study detailed a reliable and cost-effective protocol for microplastics collection and detection from the daily use of plastic products.

每日使用期间从聚丙烯婴儿喂养瓶中释放的微塑料的采样、鉴定和特征

Microplastics (MPs) are becoming a global concern due to the potential risk to human health. Case studies of plastic products (i.e., plastic single-use ...

Investigating Long-Distance Transport of Perfluoroalkyl Acids in Wheat via a Split-Root Exposure Technique

Large amounts of perfluoroalkyl acids (PFAAs) have been introduced into the soil and accumulated by plants, posing potential risks to human health. It is imperative to investigate the accumulation and translocation of PFAAs within plants. Long-distance transport is an important pathway for PFAAs transferred from the plant leaves to the edible tissues through the phloem. However, it was previously difficult to assess the translocation potential of organic contamination in a short-term exposure period. The split-root experiment provides a solution to effectively uncover the long-distance translocation of PFAAs using a hydroponic experiment, which, in this study, was carried out in two 50 mL centrifuge tubes (A and B), of which centrifuge tube A had 50 mL of one-quarter strength Hoagland sterile nutrient solution, while centrifuge tube B had the same amount of nutrient concentration, and the target PFAAs (perfluorooctane sulfonic acid, PFOS, and perfluorooctane acid, PFOA) added at a given concentration. A whole wheat root was manually separated into two parts and inserted carefully into tubes A and B. The concentration of PFAAs in the roots, shoots of wheat, and solutions in tubes A and B were evaluated using LC-MS/MS, respectively, after being cultured in an incubator for 7 days and harvested. The results suggested that PFOA and PFOS experience a similar long-distance transport process through the phloem from the shoot to the root and could be released into the ambient environment. Thus, the split-root technique can be used to evaluate the long-distance transport of different chemicals.

Investigating Long-Distance Transport of Perfluoroalkyl Acids in Wheat via a Split-Root Exposure Technique

The present protocol describes a simple and efficient method for the long-distance transport of perfluoroalkyl acids in wheat.

通过裂根暴露技术 研究 全氟烷基酸在小麦中的长距离运输

Large amounts of perfluoroalkyl acids (PFAAs) have been introduced into the soil and accumulated by plants, posing potential risks to human health. It is ...

Separation and Identification of Conventional Microplastics from Farmland Soils

Microplastics (MPs) pollution in the terrestrial environment has received increasing attention over the last decade, with increasing studies describing the numbers and types of MPs in different soil systems and their impacts on soil and crop health. However, different MPs extraction and analytical methods are used, limiting opportunities to compare results and generate reliable evidence for industry advice and policymakers. Here, we present a protocol that describes the methodology for sampling, separation, and chemical identification of conventional MPs&#160;from soil. The method is low-cost, and the materials are readily available. This enhances operational ease and may help with widespread adoption. The protocol provides detailed information on sample collection from the top 0-30 cm of soil using plastic-free utensils; simulation of different soil types through the use of various solid media (such as bentonite clay, silicon dioxide, and non-contaminated soil), with the addition of the same mass&#160;of polyethylene(PE)-MPs for subsequent quantification; density separation of plastic particles utilizing saturated sodium chloride (NaCl) solution and digestion of organic impurities in the supernatant using 4 M sodium hydroxide (NaOH) solution; quantification of particles using fluorescent microscopy after Nile Red staining; and polymer identification using micro&#160;Fourier-Transform Infrared Spectroscopy (&#956;-FTIR) or Laser-Direct Infrared (LDIR) spectroscopy. The MPs recovery rate ranged from 83% - 90% for the abovementioned media. This protocol presents an efficient method for soil MPs analysis that is optimized for feasibility, applicability, and cost-effectiveness. Moreover, the video accompanied can guide the process of analyzing the soil MPs step-by-step virtually. This study is dedicated to standardizing the methods for soil MPs analysis, enhancing the connectivity and comparability of measurements, and establishing a foundation for more standardized and scientific research.

Presented here is a method for extracting microplastics from soil and identifying their polymer types. The method has been optimized for execution, applicability, and cost-effectiveness. It lays a scientific foundation for standardizing the analytical method to identify microplastics in soils.

农田土壤中常规微塑料的分离和鉴定

Microplastics (MPs) pollution in the terrestrial environment has received increasing attention over the last decade, with increasing studies describing ...

Analysis of Organochlorine Pesticides in a Soil Sample by a Modified QuEChERS Approach Using Ammonium Formate

Currently, the QuEChERS method represents the most widely used sample preparation protocol worldwide for analyzing pesticide residues in a broad variety of matrices both in official and non-official laboratories. The QuEChERS method using ammonium formate has previously proven to be advantageous compared to the original and the two official versions. On the one hand, the simple addition of 0.5 g of ammonium formate per gram of sample is sufficient to induce phase separation and achieve good analytical performance. On the other hand, ammonium formate reduces the need for maintenance in routine analyses. Here, a modified QuEChERS method using ammonium formate was applied for the simultaneous analysis of organochlorine pesticide (OCP) residues in agricultural soil. Specifically, 10 g of the sample was hydrated with 10 mL of water and then extracted with 10 mL of acetonitrile. Next, phase separation was carried out using 5 g of ammonium formate. After centrifugation, the supernatant was subjected to a dispersive solid-phase extraction clean-up step with anhydrous magnesium sulfate, primary-secondary amine, and octadecylsilane. Gas chromatography-mass spectrometry was used as the analytical technique. The QuEChERS method using ammonium formate is demonstrated as a successful alternative for extracting OCP residues from a soil sample.

The present protocol describes the utilization of ammonium formate for phase partitioning in QuEChERS, together with gas chromatography-mass spectrometry, to successfully determine organochlorine pesticide residues in a soil sample.

使用甲酸铵的改进QuEChERS方法分析土壤样品中的有机氯农药

Currently, the QuEChERS method represents the most widely used sample preparation protocol worldwide for analyzing pesticide residues in a broad variety ...

从塑料颗粒中提取有机氯农药和塑料类型分析

摘要

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此视频中的章节

多氯联苯同系物净营养转移效率湖鳟鱼实验室估计（

表征和被动采样的应用在农药水监测

协议塑料微粒采样的海面和样品分析

海洋浮游生物和悬浮颗粒的超洁净多层采集装置

高悬浮泥沙荷载和大型漂浮碎屑水生环境中 Microplastics 的取样、分类和表征

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

每日使用期间从聚丙烯婴儿喂养瓶中释放的微塑料的采样、鉴定和特征

通过裂根暴露技术研究全氟烷基酸在小麦中的长距离运输

农田土壤中常规微塑料的分离和鉴定

使用甲酸铵的改进QuEChERS方法分析土壤样品中的有机氯农药

从塑料颗粒中提取有机氯农药和塑料类型分析

摘要

探索更多视频

此视频中的章节

多氯联苯同系物净营养转移效率湖鳟鱼实验室估计（

表征和被动采样的应用在农药水监测

协议塑料微粒采样的海面和样品分析

海洋浮游生物和悬浮颗粒的超洁净多层采集装置

高悬浮泥沙荷载和大型漂浮碎屑水生环境中 Microplastics 的取样、分类和表征

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

每日使用期间从聚丙烯婴儿喂养瓶中释放的微塑料的采样、鉴定和特征

通过裂根暴露技术 研究 全氟烷基酸在小麦中的长距离运输

农田土壤中常规微塑料的分离和鉴定

使用甲酸铵的改进QuEChERS方法分析土壤样品中的有机氯农药

通过裂根暴露技术研究全氟烷基酸在小麦中的长距离运输