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A needle trap device (NTD) was developed using an amide-based covalent-organic framework (COF), chemically bonded to silica nanoparticles. The NTD was coupled with gas chromatography-flame ionization detection (GC-FID) and employed for the headspace microextraction analysis of halogenated hydrocarbons (HHCs) in the air. The adsorbent was characterized using Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction analysis (XRD), transmission electron microscopy (TEM), and field-emission scanning electron microscopy (FE-SEM) techniques. Optimal values for the experimental variables were assessed using response surface methodology (RSM) with a central composite design (CCD), thereby reducing the number of experiments, material consumption, costs, and time. The optimal values for desorption time and temperature were obtained 5 min and 260 °C, respectively. Breakthrough volume (BtV) was studied over the range of 0.5 - 3 times the occupational exposure limit (OEL) and its optimal value was found to be 1200 mL. The optimal sampling temperature and relative humidity (RH) were obtained 20 °C, and 15 %, respectively. The limits of detection (LODs) and limits of quantification (LOQs) were ranged from 0.013 to 0.077 μg l -1 and 0.041 to 0.21 μg l -1 , respectively, with a linear dynamic range (LDR) of 0.04 to 100 μg l -1 . The method's repeatability and reproducibility (RSD %) were observed over the ranges of 5.3 - 6.4 % and 4.7 -6.9 %, respectively. A statistically validated agreement was observed between the NTD-GC-FID method and the NIOSH 1003 standard procedure for the sampling and determination of HHCs in real workplace air samples, demonstrating the reliability and accuracy of the developed approach., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

A relatively new adsorbent based on covalent organic frameworks (COFs) was employed for the first time to extract and determine Trans, trans-muconic acid (tt-MA), Mandelic acid (MA), Hippuric acid (HA), and 3-Methylhippuric acid (m-MHA) in urine. For this purpose, microextraction was performed using the packed sorbent (MEPS) method. Following the extraction process, the prepared samples were specified via the high-performance liquid chromatography-ultraviolet detector system. The precipitation polymerization was applied to synthesize the Fe 3 O 4 @TbBd nanobeads, and the morphological and dimensional structures of the products were specified with FE-SEM images. Some key variables affecting the extraction efficiency (i.e., sample volume, elution volume, condition and washing solvents, type and volume of elution solvent, extraction cycles, temperature, and pH of the sample solution) were investigated. In ideal conditions, the limit of detection (LOD) was obtained from 0.02 µg/ml for tt-MA to 0.5 µg/ml for MA. Calibration curves (at five-point) were plotted in the range 0.05-5 µg/ml for tt-MA to 1-300 µg/ml for MA (R 2  > 0.98). Moreover, intra- and inter-day precision values were 3.1-5.5 and 4.6-9.8%, respectively. The developed method was successfully employed to determine four analytes in three concentrations (low, medium, and high QCs). The results showed a satisfactory recovery (70-87%). COF-MEPS technique is a rapid, easy, user-friendly, and environment-friendly method for separating the minimum values of all BTEXs chief biomarkers from urine samples without using complicated processes and only with one adsorbent. Also, it can be a good alternative for biomonitoring the workers exposed to BTEX compounds in occupational and environmental access., (Copyright © 2022 Elsevier B.V. All rights reserved.)

Background: Rheumatoid arthritis (RA) is an autoimmune disease with systemic inflammatory arthritis. This meta-analysis was conducted to examine the association between occupational exposure to silica and the risk of developing RA among different workers., Methods: In this meta-analysis, we searched relevant published studies using major electronic databases including Scopus, PubMed, ISI Web of Science, and Google Scholar search engine up to October 2019, and the references of retrieved articles were also checked for further possible sources. A random-effects model was used to account for heterogeneity among the results of the studies using the pooled odds ratios (ORs) and their 95% confidence intervals (CIs). The Q-statistic and I 2 tests were calculated to assess heterogeneity between the studies., Results: The pooled calculation of OR indicated a significant association between occupational exposure to silica and risk of developing RA among different workers (OR = 2.59, 95% CI = 1.73 to 3.45). In addition, the pooled estimates of OR in smokers were statistically significant (OR = 2.49, 95% CI = 1.13 to 3.86)., Conclusions: The findings of the present study reveal that occupational exposure to silica may be associated with increased risk of developing RA., Competing Interests: The authors have no conflict of interest to declare., (© 2020 The Authors.)

Background: A needle trap device (NTD) was packed with Carbotrap/silica composite sorbent and applied for field sampling of halogenated volatile organic compounds (HVOCs) followed by gas chromatography/mass spectrometry (GC/MS) separation and determination., Methods: Carbotrap B, as a highly pure surface sorbent, was prepared using sol-gel method to improve its surface properties for adsorption/desorption of the target analytes. The effects of important experimental variables on the sampling and determination of trichloroethylene (thrCE) and tetrachloroethylene (tetCE) using the proposed NTD-GC/MS strategy were evaluated and optimized., Results: The results showed that sampling temperature and relative humidity interfered with sampling efficiency of the developed method and peak area responses of the analytes decreased with increasing temperature and relative humidity. The peak areas of the analytes increased with raising desorption temperature from 180 to 250 °C, and increasing desorption time from 1 to 3 min. The carryover experiments showed that the carryover effect disappeared after 3 min of desorption time. The Limits of Detection (LODs) and Limits of Quantitation (LOQs) of the analytes were in the range 0.01-0.03 and 0.05-0.09, respectively., Conclusions: The results indicated that the developed NTD-GC/MS procedure can be used as a technology with high sensitivity for the field sampling and determination of HVOCs., Competing Interests: Competing interestsThe authors declare that there is no conflict of interest regarding this paper., (© Springer Nature Switzerland AG 2019.)

In this study, two hybrid metal organic frameworks including MOF-5@ Fe 3 O 4 -NH 2 and MOF-5@ SBA-15 for the first time were synthetized and combined with microextraction by packed sorbent (MEPS) to extract of mandelic acid (MA) from urine samples. The synthetized sorbents were characterized using FE-SEM, XRD and FT-IR techniques. The important parameters in MEPS procedure including sample volume, extraction draw&#95;discard cycles, elution solvent volume and desorption draw-eject cycles were optimized using response surface methodology (RSM) with central composite design (CCD). The results indicated that the volume of elution solvent was the most important parameter in the recovery of MA by MOF-MEPS procedure. The optimized MOF-MEPS method offered an acceptable efficiency for the recovery of MA from urine samples (MOF-5@Fe 3 O 4 -NH 2 and MOF-5@SBA-15: 94.5% and 90.3%, respectively, RSD < 3.54%). The limit of detection (LOD) of MA calculated by MOF-MEPS procedure combined with high performance liquid chromatography for MOF-5@ Fe 3 O 4 -NH 2 and MOF-5@ SBA-15 were calculated to be 0.10 and 0.13 μg mL -1 , respectively. The linearity dynamic ranges (LDRs) determination of urinary MA by MOF-5@ Fe 3 O 4 -NH 2 and MOF-5@ SBA-15 were 0.2-100 and 0.2-90 μg mL -1 , respectively. The results of the present study implied that the proposed technique is a fast and sensitive procedure for extraction and determination of MA from urine samples., (Copyright © 2019 Elsevier B.V. All rights reserved.)

The purpose of this study was to develop a novel one-step method for the time-weighted average determination of 1,1-dimethylhydrazine (UDMH) in the air followed by spectrophotometric detection. For this reason, 0.1% hydrochloric acid as the absorbent was used in hollow fiber (HF) membrane for sampling of UDMH from an atmospheric standard chamber. Response surface methodology (RSM) with central composite design (CCD) was used to optimize the sampling parameters, such as flow rate and sampling time. Moreover, several analytical parameters including breakthrough (BT) volume, storage time, and carryover effect of the proposed HF were investigated. The results showed that optimal sampling rate was 9.90 mL/min. In order to validate the proposed method, it was compared with the National Institute for Occupational Safety and Health (NIOSH) 3515 method, which showed good compatibility between the two methods. Intra- and inter-day repeatability values of the HF method were in the range 0.082-0.1 and 0.091-0.12, respectively, and the limits of detection (LODs) and limits of quantitation (LOQs) were 0.002 and 0.006 ng/mL, respectively. The storage time of the proposed HF was 7 days at 2 °C. These results demonstrated that the one-step HF membrane offered a high sensitivity for sampling of UDMH in air.

Mandelic acid (MA) is a major metabolite of ethylbenzene and styrene. For the first time, a selective, fast, and easy-to-use procedure was developed for the determination of MA in urine samples. The new procedure is based on MIMEPS, the combination of a molecularly imprinted polymer (MIP) and microextraction by packed sorbent (MEPS). High-performance liquid chromatography with ultraviolet detection (HPLC-UV) was used for the separation and determination of MA. The bulk polymerization method was used to synthesize the MIP, and the MIP and non-imprinted polymer (NIP) were characterized by Fourier transform infrared spectroscopy. The selectivity of the MIP was investigated in the presence of interferents. In addition, we investigated the various parameters that affect the performance of the MEPS, including the pH of the sample, the number of extraction cycles, sample volume, and the types and volumes of the washing and elution solvents. A six-point calibration curve was obtained in the range of 0.2-20 µg/mL (R 2  = 0.9994). The extraction recovery was more than 88.8%. The limit of detection and the limit of quantitation were 0.06 and 0.2 µg/mL, respectively. The intra- and inter-day precisions were in the range of 3.6-4.7% and 3.8-5.1%, respectively. The accuracy was -8.4 to -11.1%. The optimized procedure was selective, sensitive, and rapid, and it was both user friendly and environmentally friendly. The sample preparation process took only about 5 min, so the MIMEPS-HPLC-UV procedure is recommended as an alternative for the biomonitoring of workers exposed to ethylbenzene and/or styrene.

In the original publication of the article, there is an error in Fig. 2c. The authors would like to correct this error and the corrected version of Fig. 2c is as follow.

trans,trans-Muconic acid (tt-MA) has been introduced as biological exposure index for workers exposed to benzene. In the present study, for the first time, a novel and easy-to-use analytical method based on molecularly imprinted polymer (MIP) in microextraction by packed sorbent (MEPS), followed by high-performance liquid chromatography with ultra-violet detection (MIMEPS-HPLC-UV) was developed to determine tt-MA in urine samples. Fourier transform infrared spectroscopy was used for MIP characterization. The imprinting effect on the MIP was also evaluated. Furthermore, various parameters that affect the MEPS performance were investigated, including extraction cycles, sample volume, as well as the type and volume of washing and elution solvents. The optimised procedure was selective, sensitive, rapid and both user- and environmentally-friendly. A seven-point calibration curve was obtained in the range of 0.015-2μg/mL (R 2 =0.9986). The extraction recovery was >89.8%. The limit of detection and limit of quantitation for tt-MA were 0.015 and 0.05μg/mL, respectively. The within- and between-day precisions, given as percent relative standard deviation, were in the range of 3.4-4.7% and 3.5-6.6%, respectively. Accuracy was -8.4 to -10.2% in urine samples. The developed method is suggested as an alternative to existing conventional SPE methods for biomonitoring of benzene-exposed subjects., (Copyright © 2017 Elsevier B.V. All rights reserved.)

For the first time, hollow-fiber liquid-phase microextraction combined with high-performance liquid chromatography-ultraviolet was used to extract trans,trans-muconic acid, in urine samples of workers who had been exposed to benzene. The parameters affecting the metabolite extraction were optimized as follows: the volume of sample solution was 11 mL with pH 2, liquid membrane containing dihexyl ether as the supporter, 15% (w/v) of trioctylphosphine oxide as the carrier, the time of extraction was 120 minutes, and stirring rate was 500 rpm. Organic phase impregnated in the pores of a hollow fiber was extracted into 24 µL solution of 0.05 mol L(-1) Na2CO3 located inside the lumen of the fiber. Under optimized conditions, a high enrichment factor of 153-182 folds, relative recovery of 83%-92%, and detection limit of 0.001 µg mL(-1) were obtained. The method was successfully applied to the analysis of ttMA in real urine samples.

In this study, the application of a novel nanomaterial composite was investigated in two microextraction techniques of solid-phase microextraction and a needle trap device in a variety of sampling conditions. The optimum sampling temperature and relative humidity were 10°C and 20%, respectively, for both techniques with two sorbents of graphene/silica composite and polydimethyl siloxane. The two microextraction techniques with the proposed sorbent showed recoveries of 95.2 and 94.6% after 7 days. For the needle trap device the optimums desorption time and temperature were 3 min at 290°C and for SPME these measures were 1 and 1.5 min at 240-250°C for the graphene/silica composite and polydimethyl siloxane, respectively. The relative standard division obtained in inter- and intra-day comparative studies were 3.3-14.3 and 5.1-25.4, respectively. For four sample the limit of detection was 0.021-0.25 ng/mL, and the limit of quantitation was 0.08-0.75 ng/mL. The results show that the graphene/silica composite is an appropriate extraction media for both techniques. Combining an appropriate sorbent with microextraction techniques, and using these in conjunction with a sensitive analytical instrument can introduce a strong method for sampling and analysis of occupational and environmental pollutants in air., (© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

In this paper we describe the application of a needle trap microextraction device packed with graphene nanoplatelets for the sampling and analysis of perchloroethylene in dry cleaning. The study was carried out in two phases. First the parameters for the sampling and analysis of perchloroethylene by NTD were evaluated and optimized in the laboratory. Then the sampler was used to determine the levels of perchloroethylene in a dry-cleaning shop. In the laboratory phase of the study the performance of the NTD packed with the proposed sorbent was examined in a variety of sampling conditions to evaluate the technique. The technique was also compared with NTDs packed with PDMS as well as SPME with Carboxen/PDMS-coated fibers. Both the NTDs and SPME performed better at lower sampling temperatures and relative humidity levels. The post-sampling storage times for a 95% recovery of the analyte were 5, 5 and 3 days for NTD-graphene, NTD-PDMS and SPME-CAR/PDMS respectively. The optimum desorption time was 3 min for NTDs packed with either graphene or PDMS and 1 min for SPME-CAR/PDMS. The limits of detection for the GC/MS detection system were 0.023 and 0.25 ng mL(-1) for NTDs packed with graphene and PDMS and 0.014 ng mL(-1) for SPME coated with CAR/PDMS. In the second stage of the study the evaluated technique was applied to the sampling and analysis of perchloroethylene in dry cleaning. In this environment the performance of the NTD-graphene as a field sampler for PCE was similar to that of the SPME-CA/PDMS, and better than the NIOSH 1003 method which had greater measurement variations. The results show that a NTD packed with carbonic graphene nanoplatelets and used as an active exhaustive sampling technique is effective for determination of VOC and HVOC occupational/environmental pollutants in air., (Copyright © 2014 Elsevier B.V. All rights reserved.)

A green, environmental friendly and sensitive method for determination of volatile organohalogen compounds was described in this paper. The method is based on a homemade sol-gel single-walled carbon nanotube/silica composite coated solid-phase microextraction to develop for sampling and analysis of Carbon tetrachloride, Benzotrichloride, Chloromethyl methyl ether and Trichloroethylene in air. Application of this method was investigated under different laboratory conditions. Predetermined concentrations of each analytes were prepared in a home-made standard chamber and the influences of experimental parameters such as temperature, humidity, extraction time, storage time, desorption temperature, desorption time and the sorbent performance were investigated. Under optimal conditions, the use of single-walled carbon nanotube/silica composite fiber showed good performance, high sensitive and fast sampling of volatile organohalogen compounds from air. For linearity test the regression correlation coefficient was more than 98% for analyte of interest and linear dynamic range for the proposed fiber and the applied Gas Chromatography-Flame Ionization Detector technique was from 1 to 100 ngmL(-1). Method detection limits ranged between 0.09 to 0.2 ngmL(-1) and method quantification limits were between 0.25 and 0.7 ngmL(-1). Single-walled carbon nanotube/silica composite fiber was highly reproducible, relative standard deviations were between 4.3 to 11.7 percent.

This paper describes a new extraction technique with needles and a sorbent based on carbon nanotubes to analyze trace amounts of three isomers of xylenes in aqueous samples. In this research, results have been compared with one commercial sorbent. The synthesized sorbent was prepared using sol-gel technology and was packed into 20 gauge needles, and the same size needle was used for packing the commercial sorbent. In the extraction process, a purge and trap sampling methodology is developed, so purging and trapping cycles were performed by a sampling pump. Optimized conditions for standard xylene samples have been obtained, and eight urine samples from workers that were exposed to xylene in the workplace were collected and analyzed. Experimental parameters such as limits of detection and quantification were investigated, and these two parameters were <1 μg/L., (© 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

A needle trap device (NTD) packed with silica composite of multi-walled carbon nanotubes (MWCNTs) prepared based on sol-gel technique was utilized for sampling and analysis of volatile organohalogen compounds (HVOCs) in air. The performance of the NTD packed with MWCNTs/silica composite as sorbent was examined in a variety of sampling conditions and was compared with NTDs packed with PDMS as well as SPME with Carboxen/PDMS-coated fibers. The limit of detection of NTDs for the GC/MS detection system was 0.01-0.05 ng mL(-1) and the limit of quantitation was 0.04-0.18 ng mL(-1). The RSD were 1.1-7.8% for intra-NTD comparison intended for repeatability of technique. The NTD-MWCNTs/silica composite showed better analytical performances compared to the NTD-PDMS composite and had the same analytical performances when compared to the SPME-Carboxen/PDMS fibers. The results show that NTD-MWCNTs-GC/MS is a powerful technique for active sampling of occupational/environmental pollutants in air., (Copyright © 2013 Elsevier B.V. All rights reserved.)

This paper describes a new approach that combines needle trap devices (NTDs) with a newly synthesized silanated nano material as sorbent for sampling and analysis of HVOCs in air. The sol-gel technique was used for preparation of the single wall carbon nanotube (SWCNT)/silica composite as sorbent, packed inside a 21-gauge NTD. Application of this method as an exhaustive sampler device was investigated under different laboratory conditions in this study. Predetermined concentrations of each analyte were prepared in a home-made standard chamber, and the effects of experimental parameters, such as temperature, humidity, sampling air flow rate, breakthrough volume and storage time on NTD, and the sorbent performance were investigated. The proposed NTD was used in two different modes and two different injection methods, and an NTD with a side hole, a narrow neck glass liner and syringe pump assisted injection of carrier gas were applied. The NTD packed with SWCNTs/silica composite was compared to the NTD packed with PDMS and also SPME with CAR/PDMS. For four compounds, LOD was 0.001-0.01 ng mL(-1), LOQ was 0.007-0.03 ng mL(-1), and the relative standard division for repeatability of method was 2.5-6.7%. The results show that the incorporation of NTD and SWCNTs/silica composite is a reliable and effective approach for the sampling and analysis of HVOCs in air. Coupling this system to GC-MS make it more sensitive and powerful technique., (Copyright © 2012 Elsevier B.V. All rights reserved.)