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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >An innovative ultrasound assisted extraction micro-scale cell combined with gas chromatography/mass spectrometry in negative chemical ionization to determine persistent organic pollutants in air particulate matter
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An innovative ultrasound assisted extraction micro-scale cell combined with gas chromatography/mass spectrometry in negative chemical ionization to determine persistent organic pollutants in air particulate matter

机译：一种创新的超声辅助萃取微型电池与气相色谱/质谱联用进行负化学电离，以确定空气微粒中的持久性有机污染物

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New clean technologies are needed to determine concentration of organic pollutants without generating more pollution. A method to extract Persistent Organic Pollutants (POPs) from airborne particulate matter was developed using a novel technology recently patented called ultrasound assisted extraction micro-scale cell (UAE-MSC). This technology extracts, filters, collects the sample, and evaporates the solvent, on-line. No sample transfer is needed.The cell minimizes sample manipulation, solvent consumption, waste generation, time, and energy; fulfilling most of the analytical green chemistry protocol. The methodology was optimized applying a centred 2(3) factorial experimental design. Optimum conditions were used to validate and determine concentration of 16 organochlorine pesticides (OCIs) and 6 polybrominated diphenyl ethers (PBDEs). The best conditions achieved were 2 extractions with 5 mL (each) of dichloromethane over 5 min (each) at 60 degrees C and 80% ultrasound potency. POPs were determined by gas chromatography/mass spectrometry in negative chemical ionization (GC/MS-NCI). Analytical method validation was carried out on airborne particles spiked with POPs at seven concentration levels between 0.5 and 26.9 pg m(-3). This procedure was done by triplicate (N = 21). Recovery, ranged between 65.5 +/- 2.3% and 107.5 +/- 3.0% for OCIs and between 79.1 +/- 6.5% and 105.2 +/- 3.8% for PBDEs. Linearity (r(2)) was >= 0.94 for all compounds. Method detection limits, ranged from 0.5 to 2.7 pg m(-3), while limits of quantification (LOQ), ranged from 1.7 to 9.0 pg m(-3). A Bias from -18.6% to 9% for PBDEs was observed in the Standard Reference Material (SRM) 2787. SRM 2787 did not contain OCIs. OCIs recoveries were equivalent by UAE-MSC and Soxhlet methods UAE-MSC optimized extraction conditions reduced 30 times less solvent and decreased the extraction time from several hours to ten minutes, respect to Soxhlet. UAE-MSC was applied to 15 samples of particles less than 2.5 mu m (PM2.5) from three seasons (warm dry, rainy, and cold dry) collected in five sites around Mexico City. OCIs (4,4'-DDE and endrin aldehyde) concentrations ranged from
机译：需要新的清洁技术来确定有机污染物的浓度而不产生更多的污染。利用最近获得专利的一种新型技术-超声波辅助提取微型细胞（UAE-MSC），开发了一种从机载颗粒物中提取持久性有机污染物（POPs）的方法。该技术可在线提取，过滤，收集样品并蒸发溶剂。无需样品转移。样品池最大程度地减少了样品处理，溶剂消耗，废物产生，时间和能源。满足大多数分析绿色化学方案的要求。应用居中的2（3）析因实验设计对方法进行了优化。使用最佳条件来验证和确定16种有机氯农药（OCI）和6种多溴联苯醚（PBDEs）的浓度。达到的最佳条件是在60摄氏度和80％的超声强度下，在5分钟内（每次）用5 mL（每次）二氯甲烷萃取2次。通过负化学电离（GC / MS-NCI）中的气相色谱/质谱法测定POP。分析方法验证是对掺有POPs的七个浓度在0.5和26.9 pg m（-3）之间的POPs的空气传播颗粒进行的。一式三份地完成该过程（N = 21）。回收率：OCI的回收率介于65.5 +/- 2.3％和107.5 +/- 3.0％之间，多溴二苯醚的回收率介于79.1 +/- 6.5％和105.2 +/- 3.8％之间。所有化合物的线性（r（2））> = 0.94。方法检测极限范围为0.5至2.7 pg m（-3），而定量极限（LOQ）范围为1.7至9.0 pg m（-3）。在标准参考材料（SRM）2787中，PBDE的偏差为-18.6％至9％。SRM2787不包含OCI。通过UAE-MSC和Soxhlet方法，OCI的回收率相当。相对于Soxhlet，UAE-MSC优化的萃取条件可减少30倍以下的溶剂，并将萃取时间从数小时减少至十分钟。将UAE-MSC应用于在墨西哥城附近五个地点收集的三个季节（暖干，多雨和冷干）中的15个小于2.5微米（PM2.5）的颗粒样品。 OCI（4,4'-DDE和异狄氏剂醛）的浓度范围从

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