The application of pesticides (mostly insecticides and fungicides) during the tea-planting process will undoubtedly increase the dietary risk associated with drinking tea. Thus, it is necessary to ascertain whether pe...The application of pesticides (mostly insecticides and fungicides) during the tea-planting process will undoubtedly increase the dietary risk associated with drinking tea. Thus, it is necessary to ascertain whether pesticide residues in tea products exceed the maximum residue limits. However, the complex matrices present in tea samples comprise a major challenge in the analytical detection of pesticide residues. In this study, nine types of lateral flow immunochromatographic strips (LFICSs) were developed to detect the pesticides of interest (fenpropathrin, chlorpyrifos, imidacloprid, thiamethoxam, acetamiprid, carbendazim, chlorothalonil, pyraclostrobin, and iprodione). To reduce the interference of tea substrates on the assay sensitivity, the pretreatment conditions for tea samples, including the extraction solvent, extraction time, and purification agent, were optimized for the simultaneous detection of these pesticides. The entire testing procedure (including pretreatment and detection) could be completed within 30 min. The detected results of authentic tea samples were confirmed by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), which suggest that the LFICS coupled with sample rapid pretreatment can be used for on-site rapid screening of the target pesticide in tea products prior to their market release.展开更多
Porcine epidemic diarrhea virus(PEDV),as the main causative pathogen of viral diarrhea in pigs,has been reported to result in high morbidity and mortality in neonatal piglets and cause significant economic losses to t...Porcine epidemic diarrhea virus(PEDV),as the main causative pathogen of viral diarrhea in pigs,has been reported to result in high morbidity and mortality in neonatal piglets and cause significant economic losses to the swine industry.Rapid diagnosis methods are essential for preventing outbreaks and transmission of this disease.In this study,a paper-based lateral flow immunoassay for the rapid diagnosis of PEDV in swine fecal samples was developed using stable color-rich latex beads as the label.Under optimal conditions,the newly developed latex bead-based lateral flow immunoassay(LBs-LFIA)attained a limit of detection(LOD)as low as 10^(3.60) TCID_(50)/mL and no cross-reactivity with other related swine viruses.To solve swine feces impurity interference,by adding a filtration unit design of LFIA without an additional pretreatment procedure,the LBs-LFIA gave good agreement(92.59%)with RT-PCR results in the analysis of clinical swine fecal samples{n=108),which was more accurate than previously reported colloidal gold LFIA(74.07%)and fluorescent LFIA(86.67%).Moreover,LBs-LFIA showed sufficient accuracy(coefficient of variance[CV]<15%)and stable(room temperature storage life>56 days)performance for PEDV detection,which is promising for on-site analysis and user-driven testing in pig production system.展开更多
The ion chromatography combined solid phase extraction (SPE) method was developed for the analysis of low concentration haloacetic acids (HAAs), a class of disinfection by-products formed from chlorination of hosp...The ion chromatography combined solid phase extraction (SPE) method was developed for the analysis of low concentration haloacetic acids (HAAs), a class of disinfection by-products formed from chlorination of hospital wastewater. The monitored HAAs included monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, dibromoacetic acid and trichloroacetic acid. The method employed a sodium hydroxide eluent at a flow rate of 0.8 ml/min, electrolytically generated gradients, and suppressed conductivity detection. To analyze the HAAs in real hospital wastewater samples, C18 pretreatment cartridge was utilized to reduce samples' turbidity. Preconcentration with SPE and matrix elimination with treatment cartridges were investigated and found to be able to obtain acceptable detection limits. Linearity, repeatability and detection limits of the above method were evaluated. The detection limits of monobromoacetic acid and dibromoacetic acid were 2.61 μg/L and 1.30 μg/L, respectively, and the other three acids are ranging from 0.48 to 0.82μg/L under 25-fold preconcentration. When the above optimization procedure was applied to three hospital wastewater samples with different treatment processes in Tianjin, it was found that the dichloroacetic acid was the major compound, and the growth ratios of the HAAs after disinfection by sodium hypochlorite were 91.28%, 63.61% and 79.50%, respectively.展开更多
Organophosphate esters(OPEs), used as flame retardants and plasticizers, are widely present in environmental waters. Development of accurate determination methods for trace OPEs in water is urgent for understanding ...Organophosphate esters(OPEs), used as flame retardants and plasticizers, are widely present in environmental waters. Development of accurate determination methods for trace OPEs in water is urgent for understanding the fate and risk of this class of emerging pollutants. However, the wide use of OPEs in experimental materials results in blank interference, which influences the accuracy of analytical results. In the present work, blank contamination and recovery of pretreatment procedures for analysis of OPEs in water samples were systematically examined for the first time. Blank contaminations were observed in filtration membranes, glass bottles, solid phase extraction cartridges, and nitrogen blowing instruments. These contaminations could be as high as 6.4–64 ng/L per treatment. Different kinds of membranes were compared in terms of contamination levels left after common glassware cleaning, and a special wash procedure was proposed to eliminate the contamination from membranes. Meanwhile, adsorption of highly hydrophobic OPEs on the inside wall of glass bottles was found to be 42.4%–86.1%, which was the primary cause of low recoveries and was significantly reduced by an additional washing step with acetonitrile. This work is expected to provide guidelines for the establishment of analysis methods for OPEs in aqueous samples.展开更多
Biological sample pretreatment is an important step in biological sample analysis. Due to the diversity of biological matrices, the analysis of target substances in these samples presents significant challenges to sam...Biological sample pretreatment is an important step in biological sample analysis. Due to the diversity of biological matrices, the analysis of target substances in these samples presents significant challenges to sample processing. To meet these emerging demands on biopharmaceutical analysis, this paper summarizes several new techniques of on-line biological sample processing: solid phase extraction, solid phase micro-extraction, column switching, limited intake filler, molecularly imprinted solid phase extraction,tubular column, and micro-dialysis. We describe new developments, principles, and characteristics of these techniques, and the application of liquid chromatography–mass spectrometry(LC–MS) in biopharmaceutical analysis with these new techniques in on-line biological sample processing.展开更多
In this study,seven pretreatment methods for chromium speciation in tanned leather were evaluated:acidic miner‑alization,ethylenediaminetetraacetic acid(EDTA)extraction,diethylenetriaminepentaacetic acid(DTPA)extracti...In this study,seven pretreatment methods for chromium speciation in tanned leather were evaluated:acidic miner‑alization,ethylenediaminetetraacetic acid(EDTA)extraction,diethylenetriaminepentaacetic acid(DTPA)extraction,alkaline extraction(NH 4 OH),ammonium nitrate extraction(NH 4 NO 3),water extraction,and phosphate buffer extrac‑tion.Acidic mineralization permitted the decomposition of the organic matter and ensured the complete digestion of leathers,giving access to the total content of chromium in each sample using inductively coupled plasma‑atomic emission spectrometry(ICP‑AES).From all the extractant media tested,EDTA proved to be the most efficient,allowing the extraction of Cr(VI)and Cr(III)as a Cr(III)‑EDTA complex,quantitatively.Method validation is presented for EDTA extraction and direct mineralization.For the EDTA extraction,method detection limit(MDL)and method quantifica‑tion limit(MQL)for total Cr in leather were 3.4 ppb and 11.2 ppb(µg of total Cr per L of extraction solution),respec‑tively.Due to the lack of leather certified reference materials(CRMs)for Cr(VI),accuracy was evaluated by spiking leather samples with a Cr(VI)solution.The spike recovery of EDTA microwave assisted extraction ranged from 91.0 to 108.6%.Interday precision was also evaluated and all variation coefficients were below 5%,for both mineralization and EDTA extraction.This article provides an efficient procedure to extract quantitatively chromium from leather,while maintaining the speciation,which can be further followed by ion chromatography‑inductively coupled plasma‑mass spectrometry(IC‑ICP‑MS).展开更多
A simple and rapid dispersive liquid–liquid microextraction(DLLME)technique coupled with gas chromatography–ion trap mass spectrometry(GC–MS)was developed for the extraction and analysis of methamphetamine(MA),peth...A simple and rapid dispersive liquid–liquid microextraction(DLLME)technique coupled with gas chromatography–ion trap mass spectrometry(GC–MS)was developed for the extraction and analysis of methamphetamine(MA),pethidine(PD),ketamine(KT)and tramadol(TD)from human urine.In this study,different parameters affecting the extraction process such as the type and volume of extraction solvent,type and volume of disperser solvent,extraction time and pH value and salt effect were studied and optimized.Under optimized conditions,the enrichment factor ranged from 185 to 226 and the average recovery ranged from 80.45%to 95.55%.The linear range was 10.0–1000.0 mg/L,the limit of detection and quantitation were in the range 0.43–1.96 mg/L and 1.44–6.53 mg/L,respectively.The relative standard deviations were in the range 1.98%–3.90%(n=7).The obtained results show that DLLME combined with GC–MS is a fast and simple method for the determination of MA,PD,KT and TD in human urine.展开更多
Grain size analysis is a common method in the study of sedimentology. For the consolidated sedimentary rocks, the traditional methods are rock slice observation and image analysis. In recent years, laser particle size...Grain size analysis is a common method in the study of sedimentology. For the consolidated sedimentary rocks, the traditional methods are rock slice observation and image analysis. In recent years, laser particle size analyzer is used widely in particle size analysis of sedimentary rock. Unlike the pretreatment of loose samples, the rock samples must be crushed, added acid to wipe out cement, and washed. However, in the step of washing, most of the fines component(less than 63 μm) in the suspended state should be inevitably lost. It will significantly affect the accuracy of particle size analysis, especially for siltstone. This paper presents a siltstone sample pretreatment method which core step is washing acid by centrifuge. Compared with traditional decantation method, the results show that the median particle size reduced 33.2 μm on average. Compared with the precipitation method which is commonly used for handling loose samples, the change of solid-liquid separation time is from 12 h to 10 min, while the average reduction of median particle size is about 15 μm. The grain size value corresponded to the cumulative volume of 10%/90% reduced 2.5 μm/20.3 μm on average. The percentage of the clay component less than 2 μm increased 2.88% on average. The fine particle(2–4 μm) and silt component(4–63 μm) increased 1.71% and 5.56% on average. Based on this method, two kinds of similar lacustrine siltstone were analyzed. They are tempestite and beach bar which are difficult to identify in the Lijin sub-depression, Dongying depression, Shengli oilfield, China. The final grain-size probability plot of tempestite is the type of “one saltation component and three suspension components”. The content of suspension components can reach to 80%–90%. The beach bar is the type of “one saltation component and two suspension components”. The content of suspension components can reach to 40%–45%. They both have the characteristics of high slope which means well sorting. But they can be distinguished based on the suspension sedimentary characteristics which were preserved by maximum degree in this kind of sample pretreatment method.展开更多
In this work,the nano-g-C_(3)N_(4)/Ui O-66-NH_(2)composite was prepared by one-step solvothermal method.The as-prepared composite was characterized by scanning electron microscopy,Brunner-Emmet-Teller measurement,ener...In this work,the nano-g-C_(3)N_(4)/Ui O-66-NH_(2)composite was prepared by one-step solvothermal method.The as-prepared composite was characterized by scanning electron microscopy,Brunner-Emmet-Teller measurement,energy dispersive spectrometer,X-ray diffraction,and Fourier transform infrared spectroscopy.By using nano-g-C_(3)N_(4)/Ui O-66-NH_(2)composite as sorbent,a dispersive solid-phase extraction coupled with high-performance liquid chromatography was developed to sensitive analysis of food colorants including tartrazine,amaranth,carmine,sunset yellow,allura red and bright blue.The experiment parameters including the amount of sorbent,adsorption time,the p H of adsorption solution,desorption time,desorption solvent,the p H of desorption solution as well as the proportion between desorption solvent and buffer solvent were investigated.Under the optimized conditions,the limits of detection(S/N=3) and limits of quantitation (S/N=10) were determined in the ranges of 0.08-0.8 and 0.2-2.0 ng/m L,respectively.With the developed sample pretreatment method,carmine and brilliant blue were determined from blueberry juice by HPLC-DAD.The contents were calculated as 1.53μg/m L and0.17μg/mL,respectively.展开更多
基金supported by grants from Shanghai Agriculture Applied Technology Development Program,China(Grant No.:2020-02-08-00-08-F01456)the Key Research and Development Program of Zhejiang Province,China(Grant No.:2020C02024-2).
文摘The application of pesticides (mostly insecticides and fungicides) during the tea-planting process will undoubtedly increase the dietary risk associated with drinking tea. Thus, it is necessary to ascertain whether pesticide residues in tea products exceed the maximum residue limits. However, the complex matrices present in tea samples comprise a major challenge in the analytical detection of pesticide residues. In this study, nine types of lateral flow immunochromatographic strips (LFICSs) were developed to detect the pesticides of interest (fenpropathrin, chlorpyrifos, imidacloprid, thiamethoxam, acetamiprid, carbendazim, chlorothalonil, pyraclostrobin, and iprodione). To reduce the interference of tea substrates on the assay sensitivity, the pretreatment conditions for tea samples, including the extraction solvent, extraction time, and purification agent, were optimized for the simultaneous detection of these pesticides. The entire testing procedure (including pretreatment and detection) could be completed within 30 min. The detected results of authentic tea samples were confirmed by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), which suggest that the LFICS coupled with sample rapid pretreatment can be used for on-site rapid screening of the target pesticide in tea products prior to their market release.
基金This work was supported by the National Key Research and Development Program of China(2016YFD0500600)the Fund for Guangdong Enterprise Science and Technology Commissioner(GDKTP2020032200).
文摘Porcine epidemic diarrhea virus(PEDV),as the main causative pathogen of viral diarrhea in pigs,has been reported to result in high morbidity and mortality in neonatal piglets and cause significant economic losses to the swine industry.Rapid diagnosis methods are essential for preventing outbreaks and transmission of this disease.In this study,a paper-based lateral flow immunoassay for the rapid diagnosis of PEDV in swine fecal samples was developed using stable color-rich latex beads as the label.Under optimal conditions,the newly developed latex bead-based lateral flow immunoassay(LBs-LFIA)attained a limit of detection(LOD)as low as 10^(3.60) TCID_(50)/mL and no cross-reactivity with other related swine viruses.To solve swine feces impurity interference,by adding a filtration unit design of LFIA without an additional pretreatment procedure,the LBs-LFIA gave good agreement(92.59%)with RT-PCR results in the analysis of clinical swine fecal samples{n=108),which was more accurate than previously reported colloidal gold LFIA(74.07%)and fluorescent LFIA(86.67%).Moreover,LBs-LFIA showed sufficient accuracy(coefficient of variance[CV]<15%)and stable(room temperature storage life>56 days)performance for PEDV detection,which is promising for on-site analysis and user-driven testing in pig production system.
基金Project supported by the Hi-Tech Research and Development Program(863) of China (No. 2003AA601130).
文摘The ion chromatography combined solid phase extraction (SPE) method was developed for the analysis of low concentration haloacetic acids (HAAs), a class of disinfection by-products formed from chlorination of hospital wastewater. The monitored HAAs included monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, dibromoacetic acid and trichloroacetic acid. The method employed a sodium hydroxide eluent at a flow rate of 0.8 ml/min, electrolytically generated gradients, and suppressed conductivity detection. To analyze the HAAs in real hospital wastewater samples, C18 pretreatment cartridge was utilized to reduce samples' turbidity. Preconcentration with SPE and matrix elimination with treatment cartridges were investigated and found to be able to obtain acceptable detection limits. Linearity, repeatability and detection limits of the above method were evaluated. The detection limits of monobromoacetic acid and dibromoacetic acid were 2.61 μg/L and 1.30 μg/L, respectively, and the other three acids are ranging from 0.48 to 0.82μg/L under 25-fold preconcentration. When the above optimization procedure was applied to three hospital wastewater samples with different treatment processes in Tianjin, it was found that the dichloroacetic acid was the major compound, and the growth ratios of the HAAs after disinfection by sodium hypochlorite were 91.28%, 63.61% and 79.50%, respectively.
基金financially supported by the National High Technology Research and Development Program of China (No.2013AA065201)Chinese Academy of Sciences (Nos.XDB14020101, YSW2013A01, YSW2013B01)
文摘Organophosphate esters(OPEs), used as flame retardants and plasticizers, are widely present in environmental waters. Development of accurate determination methods for trace OPEs in water is urgent for understanding the fate and risk of this class of emerging pollutants. However, the wide use of OPEs in experimental materials results in blank interference, which influences the accuracy of analytical results. In the present work, blank contamination and recovery of pretreatment procedures for analysis of OPEs in water samples were systematically examined for the first time. Blank contaminations were observed in filtration membranes, glass bottles, solid phase extraction cartridges, and nitrogen blowing instruments. These contaminations could be as high as 6.4–64 ng/L per treatment. Different kinds of membranes were compared in terms of contamination levels left after common glassware cleaning, and a special wash procedure was proposed to eliminate the contamination from membranes. Meanwhile, adsorption of highly hydrophobic OPEs on the inside wall of glass bottles was found to be 42.4%–86.1%, which was the primary cause of low recoveries and was significantly reduced by an additional washing step with acetonitrile. This work is expected to provide guidelines for the establishment of analysis methods for OPEs in aqueous samples.
基金supported by the National Natural Science Foundation of China(No.81102499)the Fundamental Research Funds for the Central Universities of Central South University and Hunan Science and Technology Project(No.2011SK3261)
文摘Biological sample pretreatment is an important step in biological sample analysis. Due to the diversity of biological matrices, the analysis of target substances in these samples presents significant challenges to sample processing. To meet these emerging demands on biopharmaceutical analysis, this paper summarizes several new techniques of on-line biological sample processing: solid phase extraction, solid phase micro-extraction, column switching, limited intake filler, molecularly imprinted solid phase extraction,tubular column, and micro-dialysis. We describe new developments, principles, and characteristics of these techniques, and the application of liquid chromatography–mass spectrometry(LC–MS) in biopharmaceutical analysis with these new techniques in on-line biological sample processing.
基金This work has been partially supported by University of Rouen Normandy,INSA Rouen Normandy,the Centre National de la Recherche Scientifique(CNRS),European Regional Development Fund(ERDF)NºHN0001343,Labex SynOrg(ANR‑11‑LABX‑0029)Carnot Institute I2C,the graduate school for research XL‑Chem(ANR‑18‑EURE‑0020 XL CHEM)+1 种基金Region Normandie,and Consejo Nacional de Ciencia y Tecnologia(CONACYT CVU 707668)IC instrument has been financed by RIN LabEx Milliflux Nº19E00566 and ICP/MS through Bioenairgy project(FEDER NºHN0001343).
文摘In this study,seven pretreatment methods for chromium speciation in tanned leather were evaluated:acidic miner‑alization,ethylenediaminetetraacetic acid(EDTA)extraction,diethylenetriaminepentaacetic acid(DTPA)extraction,alkaline extraction(NH 4 OH),ammonium nitrate extraction(NH 4 NO 3),water extraction,and phosphate buffer extrac‑tion.Acidic mineralization permitted the decomposition of the organic matter and ensured the complete digestion of leathers,giving access to the total content of chromium in each sample using inductively coupled plasma‑atomic emission spectrometry(ICP‑AES).From all the extractant media tested,EDTA proved to be the most efficient,allowing the extraction of Cr(VI)and Cr(III)as a Cr(III)‑EDTA complex,quantitatively.Method validation is presented for EDTA extraction and direct mineralization.For the EDTA extraction,method detection limit(MDL)and method quantifica‑tion limit(MQL)for total Cr in leather were 3.4 ppb and 11.2 ppb(µg of total Cr per L of extraction solution),respec‑tively.Due to the lack of leather certified reference materials(CRMs)for Cr(VI),accuracy was evaluated by spiking leather samples with a Cr(VI)solution.The spike recovery of EDTA microwave assisted extraction ranged from 91.0 to 108.6%.Interday precision was also evaluated and all variation coefficients were below 5%,for both mineralization and EDTA extraction.This article provides an efficient procedure to extract quantitatively chromium from leather,while maintaining the speciation,which can be further followed by ion chromatography‑inductively coupled plasma‑mass spectrometry(IC‑ICP‑MS).
文摘A simple and rapid dispersive liquid–liquid microextraction(DLLME)technique coupled with gas chromatography–ion trap mass spectrometry(GC–MS)was developed for the extraction and analysis of methamphetamine(MA),pethidine(PD),ketamine(KT)and tramadol(TD)from human urine.In this study,different parameters affecting the extraction process such as the type and volume of extraction solvent,type and volume of disperser solvent,extraction time and pH value and salt effect were studied and optimized.Under optimized conditions,the enrichment factor ranged from 185 to 226 and the average recovery ranged from 80.45%to 95.55%.The linear range was 10.0–1000.0 mg/L,the limit of detection and quantitation were in the range 0.43–1.96 mg/L and 1.44–6.53 mg/L,respectively.The relative standard deviations were in the range 1.98%–3.90%(n=7).The obtained results show that DLLME combined with GC–MS is a fast and simple method for the determination of MA,PD,KT and TD in human urine.
基金supported by the National Natural Science Foundation of China (No. 41572092)the National Science and Technology Major Project (No. 2017ZX05009-002)China Key Laboratory of Land and Resources Ministry of Shale Gas Resource Evaluation and Strategy Selection
文摘Grain size analysis is a common method in the study of sedimentology. For the consolidated sedimentary rocks, the traditional methods are rock slice observation and image analysis. In recent years, laser particle size analyzer is used widely in particle size analysis of sedimentary rock. Unlike the pretreatment of loose samples, the rock samples must be crushed, added acid to wipe out cement, and washed. However, in the step of washing, most of the fines component(less than 63 μm) in the suspended state should be inevitably lost. It will significantly affect the accuracy of particle size analysis, especially for siltstone. This paper presents a siltstone sample pretreatment method which core step is washing acid by centrifuge. Compared with traditional decantation method, the results show that the median particle size reduced 33.2 μm on average. Compared with the precipitation method which is commonly used for handling loose samples, the change of solid-liquid separation time is from 12 h to 10 min, while the average reduction of median particle size is about 15 μm. The grain size value corresponded to the cumulative volume of 10%/90% reduced 2.5 μm/20.3 μm on average. The percentage of the clay component less than 2 μm increased 2.88% on average. The fine particle(2–4 μm) and silt component(4–63 μm) increased 1.71% and 5.56% on average. Based on this method, two kinds of similar lacustrine siltstone were analyzed. They are tempestite and beach bar which are difficult to identify in the Lijin sub-depression, Dongying depression, Shengli oilfield, China. The final grain-size probability plot of tempestite is the type of “one saltation component and three suspension components”. The content of suspension components can reach to 80%–90%. The beach bar is the type of “one saltation component and two suspension components”. The content of suspension components can reach to 40%–45%. They both have the characteristics of high slope which means well sorting. But they can be distinguished based on the suspension sedimentary characteristics which were preserved by maximum degree in this kind of sample pretreatment method.
基金sponsored by the National Nature Science Foundation of China (No.22076038)Natural Science Foundation of Henan (No.202300410044)。
文摘In this work,the nano-g-C_(3)N_(4)/Ui O-66-NH_(2)composite was prepared by one-step solvothermal method.The as-prepared composite was characterized by scanning electron microscopy,Brunner-Emmet-Teller measurement,energy dispersive spectrometer,X-ray diffraction,and Fourier transform infrared spectroscopy.By using nano-g-C_(3)N_(4)/Ui O-66-NH_(2)composite as sorbent,a dispersive solid-phase extraction coupled with high-performance liquid chromatography was developed to sensitive analysis of food colorants including tartrazine,amaranth,carmine,sunset yellow,allura red and bright blue.The experiment parameters including the amount of sorbent,adsorption time,the p H of adsorption solution,desorption time,desorption solvent,the p H of desorption solution as well as the proportion between desorption solvent and buffer solvent were investigated.Under the optimized conditions,the limits of detection(S/N=3) and limits of quantitation (S/N=10) were determined in the ranges of 0.08-0.8 and 0.2-2.0 ng/m L,respectively.With the developed sample pretreatment method,carmine and brilliant blue were determined from blueberry juice by HPLC-DAD.The contents were calculated as 1.53μg/m L and0.17μg/mL,respectively.