最新刊期
卷 43 ， 期 8 ， 2024
- 摘要：Environmental Specimen Banks（ESBs） are infrastructures designed for the long-term acquisition and high-quality storage of environmental specimens. They have been playing significant role in environmental monitoring and new pollutant research. This paper reviewed the development of ESBs since the 1960s and their role in the study of new pollutants. Firstly，by introducing typical global ESBs，the mainstream functions and features of the Environmental Specimen Bank Management Systems（ESBMSs） were analyzed. Then，the essential role of ESBs in new pollutant research was expounded，including to provide an environmental sample basis for new pollutant research and to enable spatial and temporal sequence analysis and environmental behavior studies. In addition，based on the current status of ESB construction，the development tendency of ESBs in the light of present analysis technologies on new pollutants was prospected.关键词：environmental specimen bank;new pollutants;contamination monitoring;spatio-temporal analysis;retrospective analysis
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发布时间：2024-08-08 - 摘要：With the rapid increase in environmental data，machine learning has become an essential tool for environmental analysis and detection. The main goal of this review is to foster the continuous innovation of this field. In this review，the basic concepts of machine learning，common algorithms and software platforms are briefly introduced. Through a comprehensive literature analysis，it highlights the latest progress in environmental analysis and detection research that incorporates machine learning technology. Currently，research on environmental analysis and detection based on machine learning methods mainly focuses on five areas：detection of conventional environmental quality indicators，targeted and non-targeted environmental detection analysis，classification and identification of microplastics and nanoplastics，environmental behaviour of pollutants，and source apportionment. Furthermore，the paper identifies several existing deficiencies in the field. These include sample collection and pre-treatment，integration of new technologies，multimodal data fusion，and the interpretability and credibility of models in the current research. Finally，this review proposes potential future applications of machine learning methods in environmental analysis and detection，aiming to further advance and expand the application of machine learning in this field. This review can provide guidance and recommendations for researchers and decision-makers in the field of environmental analysis and detection and its intersecting areas.关键词：Environmental analytical chemistry;Environmental Detection;machine learning;emerging pollutants
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发布时间：2024-08-08 - 摘要：Endocrine disrupting chemicals（EDCs） are a group of pollutants that have drawn tremendous attention worldwide. EDCs have been detected in various media such as water，soil，air，organisms，and even in the human body，posing potential threats to ecological environment and human health. The nuclear receptor pathway is one of the important mechanisms of EDCs，where active compounds could act on nuclear receptors to regulate the transcriptional level of target genes，thereby exhibiting endocrine disrupting activity toward organism. The common biological screening methods for nuclear receptor response are in vitro or cell-free testing，which are characterized by simple operation and fast speed. The nuclear receptor-responsive bioassays can be employed to detect the endocrine-disrupting activity of pure chemicals，or identify EDCs in complex environmental media. This paper summarizes the screening criteria and current research status of EDCs，the nuclear receptor response related assays，and the application of these assays in identification of EDCs for different complex media. The future research focus of EDCs screening based on nuclear receptor activity assays and the establishment of relevant screening methods for endocrine disruptors in China is also prospected. This paper aims to provide data and technical references for the screening of emerging pollutants especially EDCs in China.关键词：endocrine disrupting chemicals;emerging pollutants;nuclear receptor activity screening assays;complex media
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发布时间：2024-08-08 - 摘要：Siloxanes have typical characteristics such as potential environmental persistence，bioaccumulation，and toxicity，and have become a type of emerging pollutants of widespread international concern in recent years. Due to their low surface tension，high thermal stability and lubricating properties，siloxanes have been widely used in daily production and life，and their production and consumption are both increasing year by year. With the large consumption of these compounds in human activities，they have been frequently detected in various environmental media，personal care products，biological matrices，silica gel products，and even food. Meanwhile，the various intermediate products formed by the degradation reactions of siloxanes in different media have gradually attracted attention. At present，the analysis methods of siloxane compounds reported in literatures were complex and diverse. And then，this article provided a review of sample collection，pretreatment methods，instrumental analysis of siloxanes，and non-targeted screening of siloxanes and their degradation products in different environmental matrices，as well as an elaboration of the problems that need to be solved in the sampling and subsequent experiments. It is hoped that this review can provide a reference for the development direction of the follow-up study of siloxanes and the selection of analytical methods.关键词：siloxanes;sampling;pretreatment;instrumental analysis;untargeted screening
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发布时间：2024-08-08 - 摘要：Research on micro/nano plastic pollution has become one of the hot topics in environmental science area because they may pose a serious threat to the environment and human health. Accurate quantitative analysis of micro/nano plastics in complex environmental media is crucial for a comprehensive understanding of the migration and transformation，biological enrichment，environmental retention and environmental effects of micro/nano plastics in the environment，as well as their risk assessment. In view of this，based on the summary of relevant research in recent years，this paper summarizes the existing quantitative tracking including metal probes labelling，fluorescence labelling，and isotope tracer labelling. In addition，we also summarize the detection technologies and instrument detection methods（i.e.，spectral analysis and mass spectrometry） for micro/nano plastics，sorts out the advantages and disadvantages of precise quantitative analysis methods for micro/nano plastics in the current environment，and the main problems and challenges faced. The knowledge gaps and future research work needed are also included in order to provide theoretical basis for establishing standard detection methods and regulatory systems for micro/nano plastics.关键词：micro/nano plastics;analysis and testing;tracing technology;recent advances
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发布时间：2024-08-08 - 摘要：In recent years，the large application of nanotechnology and nanomaterials has led to the release and accumulation of mass metal nanoparticles（MNPs） into the environment. Due to the unique physical and chemical characteristics and biological toxicity of MNPs，MNPs in the environment pose a serious threaten to the ecological environment and human health. Therefore，it is of great significance to characterize metal nanoparticles in complex matrix samples（soil，sediment，water，organisms）. Among the reported techniques for the characterization of MNPs，single particle inductively coupled plasma mass spectrometry（SP-ICP-MS） plays an important role in the separation，identification and quantification of MNPs in complex matrix samples. This review mainly introduces the principle of SP-ICP-MS analysis technology and the pretreatment methods of complex matrix samples，reviews the new progress of its application in MNPs analysis in environment science，life science and medicine in recent years，and puts forward the direction of future research and application of SP-ICP-MS technology.关键词：metal nanoparticles（MNPs）;single particle ICP-MS（SP-ICP-MS）;characterization technique;environmental medium;biological sample
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发布时间：2024-08-08 - 摘要：Halogenated polycyclic aromatic hydrocarbons（HPAHs） are emerging persistent organic pollutants that are bioaccumulative，persistent，and long-range transportable，and are mainly generated and released during industrial thermal processes. In recent years，HPAHs have been widely detected in various types of environmental media and emissions from a variety of key industries. HPAHs have dioxin-like toxicity，carcinogenicity，and DNA-damaging effects，and their contribution to the total toxicity equivalent quantity is even higher than that of dioxins in some environments，which poses a potential risk to human health. However，there is still a lack of comprehensive understanding of HPAHs. This paper introduces the sources，toxic effects and environmental distribution of HPAHs，and reviews the latest progress in HPAH pretreatment methods and detection by gas chromatography-mass spectrometry，gas chromatography-high resolution mass spectrometry，and gas chromatography-triple quadrupole mass spectrometry，with the aim of providing references to the accurate detection，traceability and treatment of HPAHs.关键词：halogenated polycyclic aromatic hydrocarbons（HPAHs）;sources;analytical methods;mass spectrometry
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发布时间：2024-08-08
Reviews
- 摘要：In this study，a method for quantitative analysis of 37 PFASs（per- and polyfluoroalkyl compounds） and qualitative analysis of 19 PFASs in fluoroelastomer and fluoroplastic products was developed based on solid phase extraction/high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）. The samples of fluoroelastomers，fluoroplastic solids and fluoroplastic textiles were extracted by ultrasonication and oscillation using 25 mmol·L-1 ammonium acetate methanol/acetonitrile（1∶1，volume ratio） solution. The samples of fluoroplastic liquids were extracted by ultrasonication and oscillation using methyltert-butylether（MTBE）. And then extract was extracted by Envi-carb and Oasis WAX cartridges，and eluted with methanol and 0.1% ammonia methanol. The target compounds were analyzed by a Acquity UPLC BEH C18 column（2.1 mm×100 mm，1.7 μm） with mobile phase consisted of 10 mmol·L-1 ammonium acetate solution and acetonitrile. The samples were detected by tandem mass spectrometry under multiple reaction monitoring（MRM） mode and quantified by internal standard method. The results showed that at spiked levels of 5 ng·g-1，10 ng·g-1 and 20 ng·g-1 （fluoroelastomer samples） and 2.5 ng·g-1，5 ng·g-1 and 10 ng·g-1 （fluoroplastic samples），the recoveries of 37 PFASs in fluoroelastomers，fluoroplastic solids，fluoroplastic textiles and fluoroplastic liquids were in the ranges of 81.3%-109%，60.9%-111%，87.8%-125%，and 88.7%-140%，and the relative standard deviations（RSDs） were 1.4%-28%，1.5%-22%，1.8%-27% and 1.4%-19%，and the method detection limits（LOD） were 0.03-0.3 ng·g-1，0.03-0.8 ng·g-1，0.02-2 ng·g-1 and 0.04-1 ng·g-1，and the method quantitation limits（LOQ） were 0.07-0.9 ng·g-1，0.08-2 ng·g-1，0.06-6 ng·g-1 and 0.1-4 ng·g-1. The recoveries of 19 PFASs ranged from 0.300%-208%，which are suitable for semi-quantitative and qualitative analysis. The method was used to detect 10 fluoroelastomer and fluoroplastic samples，and the content range of Σ37PFASs was 9.73-66.17 ng·g-1. The method is easy to operate，sensitive and accurate in quantification，which can provide technical support for the future study of PFASs residues in fluoroelastomers and fluoroplastic products，and for the improvement of China's export trade and the enforcement of domestic compliance monitoring.关键词：fluoroelastomer;fluoroplastic;per- and polyfluoroalkyl compounds（PFASs）;high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）;solid phase extraction（SPE）
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发布时间：2024-08-08 - 摘要：Benzophenone-3（BP-3） is a widely used organic ultraviolet filter. Owing to its environmental contamination and potential toxicity to organisms，rapid and convenient detection of BP-3 is needed. Herein，a microfluidic paper-based analytical device（μPAD） has been developed by integrating biomimetic composites with paper chips. The biomimetic composite consists of nanozyme and molecularly imprinted polymer（MIP），which act as the catalyst for generating signals and the recognition unit of the μPAD，respectively. In particular，the nanozyme with peroxidase activity is a dual-metal organic gel（Fe/Ru-MOG） synthesized in a simple and gentle manner and further doped with MIP via bulk polymerization. The obtained Fe/Ru-MOG@MIP-μPAD is employed for determination of BP-3 through a double-signal outputs including chemiluminescence（CL） and colorimetry. As the specific binding of BP-3 by the MIP weakens the catalytic ability of Fe/Ru-MOG towards H2O2，CL intensities decrease together with the change of colorimetric signals. Both signals were recorded by in-situ taking photos of the detection region using a mobile phone，followed by conversion to gray values for quantification. The dual signals demonstrate a good linearity within concentration ranges of 1×10-9-1×10-7 mol/L（CL） and 3×10-9- 0.9×10-7 mol/L（colorimetry），and detection limits as low as 1.63×10-10 mol/L（CL） and 1.64×10-10 mol/L（colorimetry）. The novel μPAD exhibits admirable selectivity and reliability in analysis of real samples including soil，river water and tap water. It is fair to conclude that this platform，serving as a portable and cost-effective tool，will play an important role in fast and on-site detection of BP-3.关键词：benzophenone-3;molecularly imprinted polymers;metal-organic gel;chemiluminescence-colorimetric method;microfluidic paper chip
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发布时间：2024-08-08 - 摘要：A method for analysis of the bioaccumulation and tissue distribution of per- and polyfluoroalkyl substances（PFASs） in zebrafish using ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） was established. Zebrafishes were exposed to perfluorooctane sulfonate（PFOS），perfluorooctanoic acid（PFOA），perfluorohexanesulfonic acid（PFHxS），and perfluorohexanesulfonic acid（PFDA） for durations of 7，21，and 28 days at a concentration of 100 μg/L for each analyte. After exposure，various tissues and organs from the zebrafish were isolated，extracted with methanol，and subsequently analyzed using UPLC-MS/MS under negative ion multiple reaction monitoring（MRM） mode. The results showed that there were good linear relationships in the range of 1-200 μg/L for four PFASs，with a correlation coefficient（r） not less than 0.997 4. The limits of detection（LODs） and limits of quantitation（LOQs） of the method were 0.072-0.152 ng/g and 0.287-0.609 ng/g，respectively. After being exposed to four kinds of PFASs，the zebrafish's organs will all be polluted by these four pollutants. Among the four PFASs，both PFDA and PFOS showed relatively higher accumulation levels in the organs of zebrafish. PFOA accumulates mainly in high amounts in the intestine and liver. PFHxS shows the lowest accumulation in zebrafish，with its relative contribution to the total content of the four pollutants in various organs being less than 13%. This study provides a scientific basis for elucidating the environmental behavior and ecological risk of PFASs within aquatic organisms.关键词：UPLC-MS/MS;zebrafish;PFASs;bioaccumulation;tissue distribution
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发布时间：2024-08-08 - 摘要：A liquid-liquid extraction based ultra-high performance liquid chromatography-high resolution mass spectrometry（UPLC-HRMS） method was developed for the determination of 5 emerging contaminants of p-phenylenediamine quinones（PPD-Qs） in human urine. The process of sample pretreatment and parameters of both chromatography and mass spectrometry were optimized in detail. Using 6PPD-Q-D5 as an internal standard，the method established in this study had a good linear relationship in the range of 0.01-50 ng/mL，whereas the linear correlation coefficients were greater than 0.999，and the detection limits of the method（LODs） were as low as 2.4-7.5 pg/mL. The matrix effects of the five PPD-Qs in urine samples were detected at 81.3%-110%. The average recoveries were 80.5%-114%，and intra-day and inter-day relative standard deviations（RSDs） were less than 11%. The method was applied to the determination of 5 PPD-Qs in human urine samples，and the mean concentrations of 5 PPD-Qs ranged from 0.04 ng/mL to 1.06 ng/mL. The method in our study has the advantages of simple operation，high sensitivity，and good repeatability，which is suitable for the determination of PPD-Qs in human urine.关键词：p-phenylenediamine（PPDs） antioxidants;p-phenylenediamine quinones（PPD-Qs）;emerging contaminants;UPLC-HRMS;urine
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发布时间：2024-08-08 - 摘要：Per- and polyfluoroalkyl substances（PFASs） are ubiquitous in various environmental media and have become one of the most concerning new pollutants globally due to their bioaccumulation，persistence and potential toxicity. The pollution status in urban rivers is complex in sources and greatly influenced by the surrounding functional zones and seasons. Therefore，the pollution characteristics of new pollutants such as PFASs require further investigation. This study selected the Guangzhou section of the Pearl River as the study area and investigated the spatial distribution and seasonal variations of 16 PFASs in water samples collected in July 2020. The total concentrations of PFASs in water of the Guangzhou reach of the Pearl River were （77.7 ± 38.3） ng/L（17.9-164 ng/L）. The concentrations of PFASs in the main stream were higher than those in the tributaries，and the concentrations significantly decreased from the middle and upper sections near the city to the lower sections near the estuary. The concentrations of PFASs in the rainy season were significantly lower than those in the dry season，and the compositions also changed to some extent. Perfluorooctanoic acid（PFOA） accounted for the largest proportion in both the dry and rainy seasons，but the proportions of perfluorobutane sulfonic acid（PFBS），perfluorooctane sulfonic acid（PFOS），and perfluorohexanoic acid（PFHxA） increased in the rainy season，while the proportions of PFOA and perfluorobutanoic acid（PFBA） decreased. The proportions of short-chain PFASs increased slightly，and the proportions of short-chain PFASs in water from the 70% of the sampling sites were higher in the rainy season than in the dry season. This study provides fundamental data for assessing PFASs pollution in the aquatic environment.关键词：Pearl River;aquatic environment;per- and polyfluoroalkyl substances;distribution characteristics;occurrence;high-performance liquid chromatography-tandem mass spectrometry
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发布时间：2024-08-08 - 摘要：In the present study，a cleanup method using a combination of dialysis and gel permeation chromatography（GPC） was developed to remove lipids as well as natural hormones from biological samples with the Asian clam（Corbicula fluminea） as the model organism. To effectively screen new pollutants across different categories in biological samples，the procedures of sample extraction，dialysis，and GPC separation were optimized. This method effectively removed lipids and other endogenous interferences from biological samples while retaining a broad range of new pollutants. We selected 35 contaminants with diverse physicochemical properties（logKow ranging from -1.30 to 8.41） and evaluated their recoveries after each processing step and measured the lipid contents throughout the entire cleanup procedure. The optimized extraction method was to use accelerated solvent extraction（ASE） with a mixture of hexane，acetone and dichloromethane（2∶2∶1，volume ratio） and acetonitrile，sequentially. The extracts were subjected to four rounds of dialysis，and then were purified using GPC. Depending on their physicochemical properties，target analytes were analyzed by gas chromatography-mass spectrometry（GC-MS） or liquid chromatography-tandem mass spectrometry（LC-MS/MS）. Furthermore，a vanillin-phosphoric acid method was applied to measure lipid content after each purification step. At the same time，removal efficiency of the interferences was also verified using chromatography-mass spectrometry analyses in scan mode. Results after the combined dialysis and GPC treatment showed the residual lipid content in sample extraction was less than 1.06%. The elution time for target analytes in GPC was determined to be between 8 to 20 min. Average recoveries was 55.1%±13.0%，with relative standard deviations of 1.4%–9.2%. In conclusion，the developed method effectively removed lipids and some endogenous substances from clam extracts. Meanwhile，the recoveries of all target analytes have met the requirements for trace environmental sample analysis，showing the feasibility of using this method to prepare biota samples for non-target analysis.关键词：biota sample;dialysis;gel permeation chromatography;cleanup;non-target analysis
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发布时间：2024-08-08 - 摘要：Microplastics have been widely found in natural environment and may pose potential exposure risks to ecosystems and human health. Most of researches focuses on the fate of microplastics in aquatic environment，while a few studies were related to behaviors of microplastics in soil. The present study was conducted to examine the impacts of microplastics（polyethylene（PE） and polylactic acid（PLA）） on microbial communities and arsenic transformation in arsenic-contaminated soils. Results indicate that both types of microplastics enhanced the abundance of microbial species in the soil. Compared to control group，the proportion of bioavailable arsenic species were greater in the soil + PLA groups. Both types of microplastics would increase the arsenate gene copies in soil at 6 and 12 d，promoting the reduction of bioavailable pentavalent arsenic to trivalent arsenic. The present study found that microplastics could affect the proportions of bioavailable arsenic in soil，providing data for subsequent research.关键词：microplastics;heavy metal;microorganism;soil;arsenic speciation transformation
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发布时间：2024-08-08 - 摘要：Since pets and humans are in the same environment，analyzing the concentrations of per- and polyfluoroalkyl substances（PFAS） in pet fur and evaluating pet exposure to PFAS can reflect human exposure to a certain extent，which is important for risk assessment. In this study，extraction conditions in the pretreatment process were optimized，and a high performance liquid chromatography-tandem mass spectrometry combined with solid phase extraction（SPE/HPLC-MS/MS） method was established for the detection of 24 PFAS including the 6∶2 chlorinated polyfluoroalkyl ether sulfonic acid（6∶2 Cl-PFESA） and sodium p-perfluorous nonenoxybenzene sulfonate（OBS） in pet fur. The samples were ultrasonically extracted with acetonitrile two times，and then the extracts were cleaned up by weak anion exchange（WAX） cartridges. Finally，the eluent were collected and concentrated for the detection of PFAS by HPLC-MS/MS. The instrument detection limits（LODs） and method detection limits（MDLs） ranged from 0.005-0.136 ng/mL and 0.009-0.273 ng/g，respectively. The recoveries of 24 PFAS in pet fur were 66.2%-110% and the relative standard deviations（RSDs） were 1.5%-21%. The optimized method was applied to detect PFAS in 52 pet fur samples. The results showed that 24 PFAS were detected with detection rates ranging from 3.8% to 98.1%. The total contents of 24 PFAS ranged from 0.89-17.94 ng/g，with a mean content of 5.02 ng/g. This method has the advantages of high sensitivity，good stability，and satisfactory results can be obtained when applied to the analysis of PFAS in pet fur.关键词：per- and polyfluoroalkyl substances;pet fur;solid phase extraction;high performance liquid chromatography-tandem mass spectrometry
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发布时间：2024-08-08 - 摘要：A detection method for 26 organophosphate esters in serum was established using ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. After precipitation of protein with acetonitrile，the serum sample was purified by HMR solid phase extraction column，and the purified liquid nitrogen was blown to near dryness. After redissolving in methanol，it was detected on the machine. With 5 mmol/L ammonium acetate aqueous solution and methanol as mobile phase，the target substances were separated by C18 chromatographic column. The mass spectrum was detected by electrospray ion source（positive ion mode），multi reaction monitoring mode and stable isotope internal standard method. The results showed that the 26 organophosphate esters had a good linear relationship within the corresponding mass concentration range（r2>0.997），with detection limits of 0.024 ng/mL to 0.146 ng/mL and quantification limits of 0.079 ng/mL to 0.483 ng/mL. The spiked recoveries of serum sample is 85.7% to 115%，with relative standard deviations of 4.5% to 12%. This method was used to detect actual serum samples，and two types of organophosphate esters were detected. This method is easy to operate，highly sensitive，and has good precision，which is suitable for the trace detection of organophosphate esters in large quantities of serum samples.关键词：organophosphate esters;serum;ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）;solid phase extraction
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发布时间：2024-08-08 - 摘要：This study compared the tolerance and accumulation differences of 16 common pak choi（Brassica parachinensis L.） varieties towards perfluorooctanoic acid（PFOA） and its substitute hexafluoropropylene oxide dimer acid（HFPO-DA）. Among these varieties commonly cultivated in agriculture，high-accumulating crop varieties（HACV） and low-accumulating crop varieties（LACV） were identified. The bioconcentration factor of PFOA and HFPO-DA in HACV（ZS1P）（94.7 and 51.6，respectively） were 1.3 and 1.7 times higher than those in LACV（HQ2H）（72.9 and 30.2，respectively）. Mechanism study showed that lower transpiration and higher lipid content resulted in lower PFOA and HFPO-DA accumulation in LACV. Subcellular analysis indicated that pak choi with higher proportions of PFOA and HFPO-DA in their cell walls，nucleus，and chloroplasts potentially limit the transfer of pollutants to shoots. This study screened pak choi varieties with high and low accumulating per- and polyfluoroalkyl substances and revealed the mechanism from the perspective of physiological and biochemical，which can provide guidance for agricultural cultivation to mitigate the exposure risk of persistent organic pollutants in crops.关键词：emerging per- and polyfluoroalkyl substances;perfluorooctanic acid;UPLC-MS/MS;selection of pak choi varieties
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发布时间：2024-08-08 - 摘要：Microplastics，as an emerging pollutant that received increasing attention，have been confirmed to exist widely around the world and pose risks to both environment and human health. The various characteristics of microplastics lead to diverse analytical techniques，which has limited the consistent comparability of data between different studies. With the application of mass spectrometer in microplasitcs analysis，the mass concentration showed advantages in the comparability of different research data and has been used for the evaluation of occurrence level in different environmental matrices. In this study，a qualitative and quantitative analysis method for polyethylene（PE），polypropylene（PP），polystyrene（PS），polyvinyl chloride（PVC），polyethylene terephthalate（PET），and polycarbonate（PC） microplastics was developed based on the thermogravimetric analysis/infrared spectroscopy-gas chromatography-mass spectrometer（TGA/FTIR-GC-MS）. TGA monitors the thermal stability and volatile compounds of materials by recording mass loss as a function of temperature or time. FTIR could provide functional information of chemical structure. GC-MS could identify and quantify the pyrolysis products. As a comprehensive instrument platform，TGA/FTIR-GC-MS can achieve triple analysis of microplastics combing thermal decomposition kinetic information，spectral information and mass spectrum information. After detailed method optimization，the detection limits of the quantitative analysis method（LODs） were 0.03-1.11 μg. The recoveries were 80.4%-93.3% and the relative standard deviations（RSDs） obtained from spiked experiments were 4.0%-12%（n=3） for all six plastics. To further evaluate the method performances，pine needles，which are good passive biological sampler for monitoring organic pollutants，were analyzed as field sample matrices. A total of 12 pine needle samples were collected from different areas in China，such as Wuyi Mountain，Qinghai Lake，Yangshuo，Guangxi，and Greater Hinggan Mountains. All samples were carefully washed to remove interferes during the sampling and storage. The pine needles were then digested using tetramethylammonium hydroxide pentahydrate（TMAH） and analyzed using the developed method. The results showed that the concentrations of detected microplastics ranged from 0.01 μg∙mg-1 to 3.15 μg∙mg-1 which could be an indicator for local pollution status. The detection frequency（DF） was as follows：PE，PP and PS（100%），PET（92%），PC（60%），PVC（8%）. The relative high DF suggested the possible enrichment of microplastics from environment matrix to plants，which deserves careful attentions. Meanwhile，the results also indicated that the developed method could provide satisfying capacity for complex environmental matrices analysis. This work could provide practical analysis technical for pollution assessment and environmental behavior research of microplastics.关键词：TGA/FTIR-GC-MS;microplastics;pine needles;quantitative analysis
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发布时间：2024-08-08 - 摘要：An analytical method based on high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） was established for the simultaneous detection of 22 neonicotinoid pesticides（NEOs） and their metabolites in human urine. Urine was extracted by liquid-liquid extraction after enzymatic hydrolysis，pH adjusted by formic acid，and then separated by HSS T3 column. Gradient elution was performed with （0.1% formic acid+5 mmol/L ammonium formate）/water-acetonitrile as mobile phase. The samples were scanned simultaneously in positive/negative ion mode，detected in multiple reaction monitoring（MRM） mode，and quantized by internal standard method. The results showed that there was a good linear relationship between the 22 NEOs and their metabolites in the mass concentration ranges（r2>0.995 0）. The detection limit and quantitation limit of the method were 0.05-0.10 ng/mL and 0.15-0.30 ng/mL，respectively. The average recoveries were 64.5%-125% at low，middle and high spiked levels. The relative standard deviations ranged from 0.10% to 12%. In addition，sample stability tests indicated that urine samples should be tested as soon as possible after collection. The method had been used to determine 54 real urine samples. All samples were detected NEOs or their metabolites. The established method is efficient and stable，and can simultaneously detect 22 NEOs and their metabolites.关键词：neonicotinoid pesticides;urine;liquid-liquid extraction;high performance liquid chromatography-mass spectrometry
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发布时间：2024-08-08 - 摘要：A method for determination of dechlorane plus derivatives in solid polymer recycled materials （recycled pulp，recycled plastics） was established by stepwise pyrolysis-gas chromatography-tandem mass spectrometry（EGA-GC-MS/MS）. Sample were cut up in advance and heated in the pyrolysis furnace. 6 dechloraneplus derivatives were evolving before polymer pyrolysis. The dechloraneplus derivatives were separated by ZB-5HT INFERNO column，and analyzed using tandem mass spectrometry employing the internal standard method and multi-reaction monitoring mode （MRM）. In this paper，pyrolysis and chromatography-mass spectrometry conditions were optimized. Under the optimized experimental conditions，a linear correlation of 6 dechlorane plus derivatives was observed between 10.0-500 μg/g，and quantitation limits were 4.5-11.4 mg/kg. Recycling pulp samples yielded recoveries ranging from 85.3%-113%，with relative standard deviations（RSDs） not higher than 6.4%. Recoveries of plastic polymer samples were 86.2%-116% with their RSDs（n=6） not higher than 7.2%. The sample can be directly injected for analysis without pre-treatment such as freezing，grinding and extraction. This method is simple，rapid and sensitive，which is suitable for qualitative analysis and determination of dechlorane plus derivatives from solid polymer regenerated raw materials.关键词：reprocessed plastic;recycled pulps;dechlorane plus derivatives;evolving gas analysis;gas chromatography-tandem mass spectrometry
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发布时间：2024-08-08 - 摘要：An atmospheric pressure gas chromatography-tandem mass spectrometry（APGC-MS/MS） method was established to simultaneously determine 8 types of polybrominated diphenyl ethers（PBDEs） and 9 types of novel brominated flame retardants（NBFRs）. Serum sample of 0.3 g was pretreated with HLB column solid-phase extraction and acidic silica gel column purification，and separated by DB-5HT capillary column（15 m×0.25 mm×0.10 μm）. PBDEs and NBFRs was quantitatively analyzed by APGC-MS/MS. The detection of PBDEs is using isotope dilution method，and the detection of NBFRs is using the internal standard method. This method was further validated using international serum standard reference material sample SRM 1958. Compared with the reference mass fraction range provided by SRM 1958，the measured concentrations of PBDEs were within the reference mass fraction range，with a relative standard deviation（RSD，n=6） of 6.1% to 18%. The low，medium，and high concentrations of NBFRs were added to the matrix for validation. The recoveries of matrix spiking ranged from 81.7% to 126%. The RSDs were between 6.2% and 18%. This method has high sensitivity and accuracy，stable performance，which meets the requirements for the determination of PBDEs and NBFRs in human serum and the method can be applied to human health risk assessment for PBDEs and NBFRs.关键词：polybrominated diphenyl ethers;novel brominated flame retardants;serum;atmospheric pressure gas chromatography-tandem mass spectrometry
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发布时间：2024-08-08 - 摘要：Utilizing electrospray extraction ionization tandem mass spectrometry（EESI-MS/MS） technology，a rapid detection method for benzo［k］tetraphene（DBA） in fresh bamboo juice extract was developed under optimized working conditions. The experiment was conducted in positive ion detection mode，with optimization of ion transfer tube temperature，spray voltage，electrospray solvent flow rate，and sample flow rate. By using a methanol solution of silver nitrate as the electrospray solvent，characteristic ions such as［DBA+Ag］+，［2DBA+ Ag］+，etc.，were formed，combined with collision-induced dissociation（CID），to rapidly qualitative and quantitative detection of DBA in fresh bamboo juice. Results demonstrated good linearity of DBA in the concentration range of 0.1-100 μg/L，with a linear correlation coefficient（r2） of 0.998 0，a method detection limit（LOD） of 0.054 μg/L，and a limit of quantitation（LOQ） of 0.179 μg/L. The spiked recovery is 81.5%-87.1% for DBA in fresh bamboo juice，with a relative standard deviation of 1.9%-3.9%. Notably，this method offers advantages such as simplified sample preparation，high accuracy，and direct and rapid detection，making it suitable for screening and analyzing DBA in fresh bamboo juice，as well as providing a technical means for the detection of other PAHs.关键词：electrospray extraction ionization tandem mass spectrometry（EESI-MS/MS）;fresh bamboo juice;benzo［k］tetraphene（DBA）;direct analysis
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发布时间：2024-08-08 - 摘要：The study focuses on plastic packaging materials for traditional Chinese medicine（TCM） decoctions，utilizing microscopic Fourier transform infrared spectroscopy to detect microplastics released from these packages. Through this research，an effective method for isolating and analyzing microplastics in the plastic packaging of TCM decoctions has been developed. The recovery results shows that the the average recovery of polyethylene（PE） and polyethylene terephthalate（PET） microplastics with sizes of 50 μm，200 μm and 5 000 μm were all over 90%，indicating that the proposed method was feasible for the analysis of microplastics released from the packaging of TCM decoction. By investigating the influencing factors such as opening method，filling temperature，storage time，aging process and different types of TCM decoction on the microplastics release from TCM decoction plastic packaging，providing a new basis for the safety assessment of TCM decoction plastic packaging，and also laying a solid foundation for subsequent in-depth research.关键词：microplastics;Chinese medicine soup;plastic packaging;Fourier transform infrared microspectroscopy
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发布时间：2024-08-08 - 摘要：To investigate the effects of PM2.5 on metabolomics in rats，SD rats were randomly divided into a control group（SC） and a PM2.5 model group（MG），with 15 rats in each group. Saline and PM2.5 suspension were injected into the trachea of rats in each group twice a week for 4 weeks，respectively. The metabolomic changes in the urine of rats in each group were examined by ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry（UPLC-Q-TOF MS），and multivariate statistical analyses were performed to explore the overall metabolomic changes. Through data analysis and database search，17 potential biomarkers were identified from rat urine samples，and the main metabolic pathways involved pentose and glucuronide interconversion，tryptophan metabolism，tyrosine metabolism，phenylalanine metabolism，purine metabolism，acetaminophen metabolism pathway，retinol metabolism and valproate metabolism pathway. PM2.5 induced damaging effects in the rats，which may be related to its disruption of normal metabolic activities in rats. The results of the present study can help to understand the toxicological mechanism of PM2.5，screen the potential biomarkers of PM2.5-exposed rats，and provide theoretical bases for further exploration of the toxic effects and pathogenic mechanisms of PM2.5.关键词：UPLC-Q-TOF MS;ambient fine particulate matter;metabolomics;urine
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发布时间：2024-08-08
Scientific Papers
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