Graphitized Carbon Black Research Articles

A High-Performance and Flexible Electrothermal Heater with Bending Tolerance from Layer-by-Layer Self-Assembled Graphite Nanoplates and Carbon Black on Paper

A High-Performance and Flexible Electrothermal Heater with Bending Tolerance from Layer-by-Layer Self-Assembled Graphite Nanoplates and Carbon Black on Paper

Dissipation and Dietary Risk Assessment of the Fungicide Pyraclostrobin in Apples Using Ultra-High Performance Liquid Chromatography-Mass Spectrometry.

The fungicide pyraclostrobin is the main measure used to control apple alternaria blotch in production. To evaluate the potential dietary risks for consumers, the dissipation and terminal residues of pyraclostrobin were investigated using ultra-high performance liquid chromatography-mass spectrometry (UHPLC-MS/MS). Pyraclostrobin in apples was extracted by acetonitrile with 2% ammonia and then purified using primary secondary amine (PSA) and graphitized carbon black (GCB). The method showed good linearity within the concentration range of 0.005-0.1 mg L-1, with a coefficient of determination (R2) ≥ 0.9958. The recoveries ranged from 96.0% to 103.8%, with relative standard deviations (RSDs) between 0.8% and 2.3%. The limit of quantification (LOQ) was 0.01 mg kg-1. Pyraclostrobin dispersible oil suspension was applied in 12 apple fields across China according to good agricultural practices (GAPs). In Beijing and Shandong, the dissipation of pyraclostrobin followed first-order kinetic equations, with a half-life of 11 days. The terminal residues ranged from <0.01 to 0.09 mg kg-1. The national estimated daily intake (NEDI) of pyraclostrobin was compared with the acceptable daily intake (ADI), resulting in risk quotient (RQc) of 80.8%. These results suggest that pyraclostrobin poses a low health risk to consumers under GAP conditions and according to recommended dosages.

Determination of hexachlorophene residue in fruits and vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry.

A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) -LC-MS/MS method was developed for the determination of hexachlorophene in fruits and vegetables. Samples were extracted by acetonitrile and then salted with an acetate buffer system. Extractants neutral alumina (Al-N), strong cation exchange silica gel bonded adsorbent (SCX) and graphitized carbon black (GCB) were used for sample purification. The method demonstrates excellent accuracy and reproducibility. Under optimized conditions, the correlation coefficients of hexachlorophene were higher than 0.995 in the range of 0.5-20 ng/mL. The limit of quantification (LOQ) was 2.0 μg/kg. The average recoveries, assessed at three spiked levels (2.0, 4.0, and 20.0μg/kg) across various matrices including cabbage, celery, tomato, eggplant, potato, radish, cowpea, chives, apple, peach, grape, citrus, bitter melon, banana and hami melon ranged from 72.0 to 100.5% with relative standard deviations from 3.2 to 9.8% (n = 6).

Assembly of primary secondary amine over magnetic graphitized carbon black material for selective cleansing of sample matrices

Pigments and organic acids are among the most common impurities in complex sample matrices. Their presence in the samples often interferes with the detection of trace analytes. This study aimed to design and develop magnetic materials (GCB/Fe3O4-PSA) for the efficient purification of organic acids and pigment impurities in sample matrices. We employed the acid modification method to enhance the modification of magnetic Fe3O4 by the primary secondary amine adsorption group (PSA), effectively boosting its adsorption performance. This modification technique not only retains the inherent adsorption characteristics of Fe3O4 but also avoids the irreversible damage to Fe3O4′s own adsorption by traditional grafting methods. Subsequently, Fe3O4-PSA and graphitized carbon black (GCB) were combined through a simple physical assembly method to prepare GCB/Fe3O4-PSA, which was used for the purification of pigments and organic acids in complex matrices. During the purification process, GCB/Fe3O4-PSA can be rapidly magnetically separated. After six reuses, the adsorption performance remains above 80 %, fully demonstrating the rapid purification ability and reusability potential of GCB/Fe3O4-PSA. Compared with unmodified Fe3O4, GCB/Fe3O4-PSA significantly enhanced the purification effect of complex matrices. Its adsorption capacities for chlorophyll and ascorbic acid increased by 276.9 % and 263.9 % respectively. After combining with the GCB/Fe3O4-PSA purification material, cathinones in complex matrix samples (tea, apples, carrots) were determined using UPLC-MS/MS. The recoveries in spiked samples ranged from 96.35 % to 104.17 %, with the RSDs < 3.02 %. Simultaneously, characterization methods such as SEM, FTIR, XRD, VSM, XPS, and BET were used to study the surface structure and chemical composition of GCB/Fe3O4-PSA. The above results highlight the outstanding performance of GCB/Fe3O4-PSA in the efficient purification of organic acids and pigments in complex matrices and also show its considerable application potential in the pretreatment of complex matrix samples.

Studies on Recovery of Performance of Fouled Nanocomposite Ultrafiltration Membranes on Cleaning after Treatment of Oil–Water Emulsions

Herein, we discussed the pure water flux recovery of carbon based nanofillers embedded polyvinyl chloride nanocomposite membranes after physical cleaning through backwashing &amp; flushing with flow reversal and after chemical cleaning using hydrochloric acid and caustic soda. The water flux recovery by backwashing is more than that by forward flushing for all the membrane but it is more effective in carbon black (CB) &amp; graphitized carbon black (GCB) carbon-based membranes than relatively hydrophilic multiwalled carbon-nanotube (MWCNT) &amp; carboxylated multiwalled carbon-nanotube (CMWCNT) based nanocomposite membranes. The highest water flux recovery was found ~96% for nanocomposite membranes by backwashing and caustic soda cleaning. The combination of backwashing and caustic soda cleaning could be the most effective method of cleaning of oil-water fouled membranes to restore the maximum water flux.

Multiresidue analysis of bat guano using GC-MS/MS

Bats are the second largest mammalian order and are an endangered species group with a strong need for contamination monitoring. To facilitate non-invasive monitoring of the ecological burden in bat populations, a multiresidue method for the simultaneous quantification of 119 analytes including pesticides, persistent organic pollutants (POPs), active pharmaceutical ingredients (APIs), polycyclic aromatic hydrocarbons (PAHs), UV blockers, plasticizers, and other emerging pollutants in bat guano with gas chromatography tandem mass spectrometry (GC-MS/MS) was developed. Sample preparation and clean-up were performed with a modified QuEChERS approach based on DIN EN 15662. The method uses 1.00 g bat guano as sample with acetonitrile and water for liquid-liquid extraction. Phase separation is assisted by citrate-buffered salting out agent. For clean-up of the extract, primary secondary amine (PSA) was combined with graphitized carbon black (GCB). The lower limits of quantification (LLOQ) ranged between 2.5 and 250 µg kg−1. Linearity was shown in a concentration range from the respective LLOQs to 1250 µg kg−1. The median of the mean recovery was 102.4%. Precision was tested at three concentrations. Method and injection precision were adequate with a relative standard deviation (RSD) below 20%. Furthermore, the comparative analysis with LC-MS/MS demonstrated the reliability of the results and provided a valuable extension of the analytical scope. As proof of concept, three guano samples from a German nursery roost of Myotis myotis were analysed. The results show a time-dependent change in contaminant concentration, highlighting the strong need for non-invasive contamination monitoring of whole bat populations.Graphical

Application of graphite carbon black assisted-laser desorption ionization-mass spectrometry for soy sauce product discrimination.

In a previous study, we developed a novel analytical method to directly and simultaneously detect taste- and odor-active compounds using graphite carbon black (GCB)-assisted laser desorption ionization mass spectrometry (LDI-MS). In this study, we aimed to evaluate food quality using a variety of soy sauces using the method to discriminate each product. Graphite carbon black-laser desorption ionization-mass spectrometry allowed the provision of hundreds of MS peaks derived from soy sauces in both positive and negative modes without any tedious sample pretreatments. Principal component analysis using the obtained MS peaks clearly distinguished three soy sauce products based on the manufacturing countries (Japan, China, and India). Moreover, this method identified distinct MS peaks for discrimination, which significantly correlated with their quantitative amounts in the products. Thus, GCB-LDI-MS analysis was established as a simple and rapid technique for food analysis, illustrating the chemical patterns of food products.

Determination of 35 prohibited pesticide residues in Saussurea costus by modified QuEChERS method based on multi-walled carbon nanotubes coupled with gas chromatography-tandem mass spectrometry

Saussurea costus, a perennial herb belonging to the Asteraceae family, is a vital ingredient in traditional Chinese medicine. Increased demands for the herb have led to its widespread cultivation in China, but the corresponding increase in pesticide use has raised concerns about pesticide residues. Such residues would affect the safety and global market potential of Saussurea costus. Thus, a simple method is crucial to detect pesticide residues. The QuEChERS technique, in combination with gas chromatography-tandem mass spectrometry (GC-MS/MS), is commonly used for residue detection. However, traditional adsorbents may be unable to purify complex herbal mixtures well, affecting accuracy and instrument performance. Choosing suitable purification materials for Saussurea costus samples with complex matrices is of significant importance. This study focused on the detection of 35 prohibited pesticides in Saussurea costus. A rapid detection method was established by combining the QuEChERS technique with GC-MS/MS and utilizing a combination of multiwalled carbon nanotubes (MWCNTs), octadecylsilane-bonded silica gel (C18), and anhydrous magnesium sulfate (MgSO4) as the purification adsorbent. The samples were extracted with acetonitrile, purified by an improved QuEChERS process, subjected to GC-MS/MS analysis in multiple reaction monitoring (MRM) mode, and quantified using the internal standard method. The purification effects of four materials (C18, MWCNTs, N-propyl ethylenediamine (PSA), and graphitized carbon black (GCB)) and their optimal dosages were investigated by considering the matrix characteristics of the samples. An orthogonal experimental design was employed to optimize the ratio of adsorbent combinations, and the optimal adsorbent combination was determined to be 450 mg of MgSO4, 400 mg of C18, and 50 mg of MWCNTs. Matrix effect (ME) evaluation of the S. costus matrix showed that 31 target compounds strongly exhibited matrix-enhancement effects. Thus, matrix-matched calibration was employed in this study. Methodological investigation revealed that the standard curves for the 35 pesticides exhibited good linearity, with correlation coefficients (r2) greater than 0.9970. The average recoveries at three spiked levels ranged from 69.6% to 126.9%, and the relative standard deviations (RSDs) for parallel groups were all less than 10%. The limits of detection (LODs) and quantification (LOQs) ranged from 0.2 to 5.4 μg/kg and from 0.6 to 18.1 μg/kg, respectively. The developed method was used to screen and detect 35 pesticide residues in 20 batches of S. costus samples, and the target compounds were detected in six batches. The proposed method is simple, sensitive, and accurate. Thus, it is suitable for the rapid screening and detection of the 35 pesticide residues in S. costus and provides technical support for the cultivation, production, and quality control of the herb.

A vortex-assisted liquid-liquid extraction followed by dispersive-solid phase extraction (VA-LLE/d-SPE) for the determination of eight benzoylphenylureas insecticides in tomatoes and cucumbers

AbstractMonitoring benzoylphenylureas (BPUs) residues in ready-to-eat vegetables is of great interest for an adequate assessment of human pesticide exposure. A rapid, inexpensive, simple, and effective method for determining 8 BPUs insecticides in tomatoes and cucumbers was developed and validated. Vortex-assisted liquid-liquid extraction (VA-LLE) followed by dispersive solid-phase extraction (d-SPE) using graphitized carbon black (GCB) for cleanup was used before LC-MS/MS analysis. Different parameters were optimized, including the type and volume of extractants, vortex time, and the type and amount of adsorbents used for cleanup. The evaluation showed that the method has excellent linearity (R2 ≥ 0.994). The recovered 8 BPUs insecticides from spiked tomato and cucumber samples at 0.01, 0.05, and 0.25 mg kg−1 ranged from 83.2 to 105.2%, with RSD of 4.9–14.6%. The limits of quantitation (LOQs) were 0.0025 mg kg−1 (0.005 mg kg−1 for lufenuron). Within-day repeatability ranged from 3.9 to 13.9%, while between-day repeatability ranged from 8.9% to 17.7%. The optimized method was used to analyze 100 samples of tomatoes and cucumbers marketed in Saudi Arabia.

Impact of Pt-Loading and Carbon Support of Pt/C Anode Catalysts on Membrane Degradation Rate in Fuel Cells

In order to clarify the effect of both the Pt-loading and carbon supports in various commercial Pt/C anode catalysts on the chemical degradation rate of polymer electrolyte membranes (PEMs) in fuel cells, the membrane lifetime and fluoride emission rate (FER) were examined in a single cell with an accelerated stress test (AST) at 90 °C, while the H2O2 production rates, j(H2O2), at the Pt/C catalysts were measured in a half cell with 0.1 M HClO4 solution at 90 °C. It was demonstrated that the PEM degradation rate decreased with decreasing amount of adsorbed hydrogen atoms (Had) at the Pt/C−PEM interface by lowering the Pt-loading and using a porous carbon support (locating Pt nanoparticles within pores). The use of a graphitized carbon black (GCB) support was found to be very effective to increase the lifetime due to it having the lowest j(H2O2), although this was accompanied by the disadvantage of decreased mass activity for the hydrogen oxidation reaction. We also found good correlations between the j(H2O2) measured in a half cell and FER, as well as lifetime in a single cell, so that the lifetime of the PEM can be estimated in a shorter time.

Rapid analysis and risk assessment of perchlorate in wild edible mushrooms from Yunnan, China

Ubiquitous perchlorate contamination has become an important food safety issue related to human health, but contamination characteristics and health risks of perchlorate in wild edible mushrooms remain unclear. In this study, a method based on dispersive solid phase extraction (d-SPE) clean-up procedure combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established for the rapid analysis of perchlorate in wild edible mushrooms. Sample pretreatment was achieved by acetonitrile extraction followed by clean-up with florisil and graphitized carbon black (GCB). The proposed method presented satisfactory linearity, accuracy, precision, negligible matrix effects, and low limit of detection (LOD) (0.15 µg/kg) and limit of quantification (LOQ) (0.5 µg/kg). The recoveries at four levels (0.5, 3, 30 and 300 µg/kg) were 93.1–108.7% with relative standard deviation ranging from 2.9% to 18.2% for mushroom samples. The validated methodology was successfully applied to detect 109 wild edible mushroom samples belonging to 8 species collected from Yunnan, China, and 95.41% of the samples were found to have detectable perchlorate contamination. Concentrations of perchlorate ranged from below LOD to 29.81 μg/kg, with a mean value of 4.11 μg/kg. The risk assessment results for perchlorate in wild edible mushrooms showed no health risks to consumers.

Optimizing the QuEChERS method for efficient monitoring of fipronil, thiobencarb, and cartap residues in paddy soils with varying properties.

This study aims to optimize the QuEChERS methodology for extracting three pesticides (fipronil, thiobencarb, and cartap) from two paddy soils with distinct characteristics. Various modifications were explored to enhance extraction efficiency, employing acetonitrile (MeCN) or ethyl acetate (EtOAc) for extraction and primary-secondary amine (PSA) and graphitized carbon black (GCB) for the clean-up. Assessment criteria included accuracy, precision, linearity, detection limits, uncertainty, and matrix effects. Results revealed that the clayey soil with lower organic carbon (OC) content (1.26%) and 100% moisture yielded the highest pesticide recoveries (113.72%, 115.73%, and 116.41% for FIP, THIO, and CART, respectively). In contrast, the silty clayey soil with higher OC content (2.91%) and 20% water content exhibited poor recoveries (< 60%). FIP and CART demonstrated better recoveries with MeCN, while THIO performed better with EtOAc under specific moisture conditions. Clean-up sorbents significantly reduced FIP and CART recoveries, with THIO recoveries less affected. Acidifying with HCl substantially improved CART recovery. EtOAc introduced a moderate to strong matrix effect for FIP and THIO, while MeCN in soils with 100% moisture resulted in a strong matrix effect for CART. The study highlighted the substantial impact of extraction conditions, pesticide properties, and soil conditions on the outcomes of the QuEChERS method. A comprehensive understanding of these interplays was deemed crucial for accurately quantifying pesticide residues in agricultural soils.

A liquid chromatography-mass spectrometry method for the enantioselective multiresidue determination of nine chiral agrochemicals in urine using an enrichment procedure based on graphitized carbon black.

Many agrochemicals are chiral molecules, and most of them are marketed as racemates or diastereomeric mixtures. Stereoisomers that are not the active enantiomer have little or no pesticidal activity and can exert serious toxic effects towards non-target organisms. Thus, investigating the possible exposure to different isomers of chiral pesticides is an urgent need. The present work was aimed at developing a new enantioselective high-performance liquid chromatography-mass spectrometry method for the simultaneous determination of nine chiral pesticides in urine. Two solid-phase extraction (SPE) procedures, based on different carbon-based sorbents (graphitized carbon black (GCB) and buckypaper (BP)), were developed and compared. By using GCB, all analytes were recovered with yields ranging from 60 to 97%, while BP allowed recoveries greater than 54% for all pesticides except those with acid characteristics. Baseline separation was achieved for the enantiomers of all target agrochemicals on a Lux Cellulose-2 column within 24min under reversed-phase mode. The developed method was then validated according to the FDA guidelines for bioanalytical methods. Besides recovery, the other evaluated parameters were precision (7-15%), limits of detection (0.26-2.21µg/L), lower limits of quantitation (0.43-3.68µg/L), linear dynamic range, and sensitivity. Finally, the validated method was applied to verify the occurrence of the pesticide enantiomers in urine samples from occupationally exposed workers.

Advanced QuEChERS Method Using Core-Shell Magnetic Molecularly Imprinted Polymers (Fe3O4@MIP) for the Determination of Pesticides in Chlorophyll-Rich Samples.

Graphitized carbon black (GCB) in the traditional QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used to remove the interfering substance chlorophyll in vegetable and fruit samples for pesticide residues determination. However, it not only adsorbs pigments, but also adsorbs some planar and aromatic pesticides. In order to solve the shortcoming, a core-shell magnetic molecularly imprinted polymer (Fe3O4@MIP) that can specifically recognize and adsorb chlorophyll was synthesized, and an advanced QuEChERS method with the Fe3O4@MIP as a purification material was developed. This advanced method presents detection that is highly sensitive, specific, and reproducible for planar and aromatic pesticides. The limits of detection (LOD) ranged from 0.001-0.002 mg kg-1, and the limit of quantification (LOQ) was 0.005 mg kg-1. The recovery for the planar and aromatic pesticides was within 70-110% with the associated relative standard deviations < 15% in leek samples by the advanced QuEChERS method. However, in the traditional QuEChERS method with GCB, the recovery of most planar and aromatic pesticides was <60%. It may also be useful for the determination of other pesticides in vegetable samples with quick and easy sample purification.

Simultaneous determination of polycyclic aromatic hydrocarbons and polychlorinated biphenyls in Pu-erh tea by dispersive solid-phase extraction coupled with GC-MS/MS

A novel method for the simultaneous determination of 13 PAHs and 18 PCBs residues in Pu-erh tea samples was established by combining GC-MS/MS with dispersive-solid phase extraction (d-SPE). Sample pretreatment procedure was achieved by NaCl addition and using acetone/ethyl acetate/n-hexane (50:30:20, v/v/v) extraction followed by d-SPE clean-up with strong cationic exchanger (SCX), primary secondary amine (PSA), polyvinylpolypyrrolidone (PVPP) and graphitized carbon black (GCB). The proposed method had good linearity in the range of 0.5–200 μg/L with correlation coefficients (R2 > 0.998). The detection limit ranges (LODs) were from 0.2 to 1.5 µg/kg. The spiked experiments in raw Pu-erh tea and ripened Pu-erh tea at 2.5–50 µg/kg concentrations showed satisfactory recoveries (70.2–114.7%) for all analytes with RSDs of < 10%. The validated methodology was successfully applied to 86 Pu-erh tea samples. No PCBs residue was more than LODs, and the detection frequency and concentration of PAHs in different types of Pu-erh tea varies greatly were found.

Development of Simultaneous Determination Method of Pesticide High Toxic Metabolite 3,4-Dichloroaniline and 3,5 Dichloroaniline in Chives Using HPLC-MS/MS.

3,4-dichloroaniline (3,4-DCA) and 3,5-dichloroaniline (3,5-DCA) are, respectively, the primary metabolites deriving from the breakdown of phenylurea herbicides and dicarboximide fungicides in both soils and plants, whose residues in vegetable products have a heightened concern considering their higher health risks to humans and greater toxicity than the parent compounds in the environment. In this study, a sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous determination of 3,4-DCA and 3,5-DCA residues in chive products based on the optimization of HPLC-MS/MS chromatographic and mass-spectrometric conditions using the standard substances and the modified QuEChERS preparation technique. The preparation efficiency of 3,4-DCA and 3,5-DCA from chive samples showed that acetonitrile was the best extractant. The combination of the purification agent graphite carbon black + primary secondary amine and the eluting agent acetonitrile + toluene (4:1, v/v) had a satisfactory purification effect. The linear correlation coefficients (R2) were more than 0.996 with the six concentration range of 0.001-1.000 mg/L for 3,4-DCA and 3,5-DCA. The limit of detection and limit of quantitation of this method was 0.6 and 2.0 µg/kg for 3,4-DCA, as well as 1.0 and 3.0 µg/kg for 3,5-DCA, respectively. The matrix effect range of 3,4-DCA and 3,5-DCA in chive tissues was from -9.0% to -2.6% and from -4.4% to 2.3%, respectively. The fortified recovery of 3,4-DCA and 3,5-DCA in chive samples at four spiked levels of 0.001-1.000 mg/kg was 75.3-86.0% and 78.2-98.1%, with the relative standard deviation of 2.1-8.5% and 1.4-11.9%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.6, 2.0, and 1.0, 3.03 for 4-DCA and 3,5-DCA, respectively. This study highlights that the analytical method established here can efficiently and sensitively detect residues of 3,4-DCA and 3,5-DCA residues for monitoring chive products. The method was successfully applied to 60 batches of actual vegetable samples from different regions.

Influence of metal salts (Al, Ca, and Mg) on the work function and hole extraction at carbon counter electrodes in perovskite solar cells

Hole transport material-free carbon-based perovskite solar cells (HTM-free C–PSCs) are recognized as a cost-effective and stable alternative to conventional perovskite solar cells. However, the significant energy level misalignment between the perovskite layer and the carbon counter electrode (CE) results in ineffective hole extraction and unfavorable charge recombination, which decreases the power conversion efficiency (PCE). Here, we report the introduction of metal salts (Al, Ca, and Mg) into graphite/carbon black (Gr/CB) CEs to modify the work function and enhance the hole selectivity of the CE. This modification leads to improved energy level alignment, efficient hole extraction, and reduced charge recombination. The PCE of the HTM-free C-PSC based on Al-modified Gr/CB as the CE material reached 9.91%, which is approximately 12% higher than that of devices employing unmodified Gr/CB CEs. This work demonstrates that by directly incorporating metal salts into the Gr/CB CE, the energy level alignment and hole extraction at the perovskite/carbon interface can be improved. This presents a viable method for enhancing the PCE of HTM-free C–PSCs.

Simultaneous Analysis of 53 Pesticides in Safflower (Carthamus tinctorius L.) by Using LC–MS/MS Coupled with a Modified QuEChERS Technique

Objective: An optimized quick, easy, cheap, effective, rugged, and safe (QuEChERS) technique was investigated and compared with the conventional QuEChERS technique for the simultaneous analysis of fifty-three pesticide residues in safflower using ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS). Method: Graphitic carbon nitride (g-C3N4) consisting of a major amount of carbon and nitrogen with a large surface area was used as a QuEChERS adsorbent instead of graphitized carbon black (GCB) for safflower extraction purification. Validation experiments were performed using spiked pesticide samples, and real samples were analyzed. Results: The linearity of the modified QuEChERS technique was evaluated with high coefficients of determination (R-2) being higher than 0.99. The limits of detection were &lt;10 μg/kg. The spiked recoveries ranged from 70.4% to 97.6% with a relative standard deviation of less than 10.0%. The fifty-three pesticides exhibited negligible matrix effects (&lt;20%). Thiamethoxam, acetamiprid, metolachlor, and difenoconazole were detected in real samples using an established method. Conclusion: This work provides a new g-C3N4-based modified QuEChERS technique for multi-pesticide residue analysis in complex food matrices.

Multivariate response surface methodology assisted modified QuEChERS method for the rapid determination of 39 pesticides and metabolites in medlar

A modified QuEChERS method coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established for residue analysis of 39 pollutants (34 commonly used multi-class pesticides and 5 metabolites) in medlar matrices (fresh, dried, and medlar juice). Samples were extracted using water with 0.1 % formic acid: acetonitrile (5: 10, v/v). The phase-out salts and five different cleanup sorbents (including N-propyl ethylenediamine (PSA), octadecyl silane bonded silica gel (C18), graphitized carbon black (GCB), Carbon nanofiber (C-Fiber) and MWCNTs) were investigated to improve the purification efficiency. The Box-Behnken Design (BBD) study was employed for an optimal solution of the volume of extraction solvent, phase-out salt, and the purification sorbents for the analytical method. The average recoveries of the target analytes in the three medlar matrices ranged from 70 % to 119 % with relative standard deviations (RSDs) of 1.0 %−19.9 %. Screening of market samples (fresh and dried medlars) collected from the major producing regions in China showed that 15 pesticides and metabolites were detected in the samples at concentrations of 0.01–2.22 mg/kg, and none of which exceeded the maximum residue limits (MRLs) set in China. The results showed that the risk of food safety by consumption of medlar products caused by the use of pesticides was low. The validated method could be used for rapid and accurate screening of multi-class multi-pesticide residues in Medlar for food safety.

Carbon based Nanofillers Embedded Fouling Resistant Polyvinyl Chloride Nanocomposite Membranes for Oil-water Separation

Herein, we discussed the development of polyvinyl chloride (PVC) based nanocomposite ultrafiltration (UF) membrane by embedment of nanofillers such as carbon black (CB), graphitized carbon black (GCB) or mesoporous carbon, multiwalled carbon-nanotube (MWCNT), carboxylated multiwalled carbon-nanotube (CMWCNT) with increased permeate flux and fouling resistance. Ultrafiltration membranes were prepared using casting solution of PVC in N, N-dimethylacetamide (DMAc) solvent with polyethylene glycol with average MW 600Da (PEG-600) as additives with and without nanofillers. Membranes prepared were characterized in terms of pure water permeability, separation of single uncharged solutes like polyethylene oxide (PEO), water contact angle and tensile strength. Membranes were tested with synthetic oily waste water (1000 ppm oil-water emulsion) followed by pure water flux recovery after cleaning by flow reversal flushing using deionized water. The product flux was observed to increase by ~35.5%, ~11.4% &amp; ~44.4% in PVC-GCB, PVC-MWCNT and PVC-CMWCNT membranes respectively than the pure PVC membranes. The flux recovery on cleaning of fouled membranes is ~56% in pure PVC membrane, whereas it is ~72%, ~74% &amp; ~80% for PVC-GCB, PVC-MWCNT and PVC-CMWCNT membranes respectively. Incorporation of the carbon based nanofillers in pure polymer matrixes not only enhances the water permeability with marginal decrease of the separation performances but also it increases mechanical strength and the fouling resistance of the membranes. The carbon fillers-based PVC nanocomposite membranes are found promising candidates for cleaning oily wastewater.