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Globally, around six billion people consume bovine milk. As in many other countries dairy plays an important role in the Indian diet. The Food Safety Standards Authority of India is continuously taking efforts to ensure the country's regulatory framework for the dairy sector meets international standards and secure human health and to promote trade. To ensure safe and nutritious milk and milk products, an integrated quality assurance system with a thorough surveillance program is a prerequisite. This paper outlines the risk assessment principles before listing various chemical and microbiological hazards in the dairy supply chain, discusses examples with successful dairy supply chains, suggests analytical approaches for regulatory control, and gives recommendations for an effective surveillance plan. First of its kind, the paper may contribute to the development of an integrated milk quality and safety surveillance system in India, and may also serve as guidance for other developing nations. • FSSAI strives to ensure quality and food safety in the dairy sector. • India aims to upgrade its regulatory framework to meet international standards. • Examples of structured surveillance systems in several dairy supply chains are shown. • Recommendations for building a well-planned surveillance system in India are given. [ABSTRACT FROM AUTHOR]

Monte Carlo (MC) methods have been widely used to solve eigenvalue problems in complex nuclear systems. Once a stationary fission source is obtained in MC simulations, the sample mean of many stationary cycles is calculated. Variance or standard deviation of the sample mean is needed to indicate the level of statistical uncertainty of the simulation and to understand the convergence of the sample mean. Current MC codes typically use sample variance to estimate the statistical uncertainty of the simulation and assume that the MC stationary cycles are independent. However, there is a correlation between these cycles, and estimators of the variance that ignore these correlations will systematically underestimate the variance. This paper discusses some statistical properties of the sample mean and the asymptotic variance and introduces two novel estimators based on (a) covariance-adjusted methods and (b) bootstrap methods to reduce the variance underestimation. For three test problems, it has been observed that both new methods can improve the estimation of the standard deviation of the sample mean by more than an order of magnitude. In addition, some interesting patterns were revealed for these estimates over the spatial regions, providing additional insights into MC simulations for nuclear systems. These new methodologies are based on post-processing the tally results and are therefore easy to implement and code agnostic. [ABSTRACT FROM AUTHOR]

Cancer chemotherapy suffers from selectivity and undesired toxicity of the drugs. Since zinc is a biocompatible tracer element and cysteine derivatives are used in cancer chemoprevention, we intend to develop a complex of zinc and cysteine-derivatives as potent, non-toxic anticancer agents. Herein, we synthesized and characterized cysteine based ligand, 2-[(2-Hydroxy-3-methoxy-benzylidene)-amino]-3-mercapto-propionic acid and its Zn-complex, which are found to be non-toxic towards normal human PBMC. Data also revealed that only Zn-complex exhibited remarkable apoptosis in drug-sensitive CCRF-CEM and multidrug-resistant CEM/ADR5000 cancer cells as assessed by MTT, Cell cycle and AnnexinV binding assay. Moreover, Zn-complex altered ROS and GSH level of the respective cell lines. Finally, treatment of Zn-complex in Swiss albino mice did not show any systemic toxicity in preliminary trials in normal mice and remarkably increased the life-span of EAC bearing mice. In conclusion, the synthesized Zn-complex may be developed for efficacious, multidrug resistance reversal, non-toxic chemotherapeutic agents in future. [ABSTRACT FROM AUTHOR]

Vanadium compounds are well known for their therapeutic interventions against several diseases. Various biochemical attributes of vanadium complexes inspired us to evaluate the cancer cell killing efficacy of the vanadium complex, viz., vanadyl N-(2-hydroxyacetophenone) glycinate [VO(NG) 2 ]. Previously we showed that VO(NG) 2 is an effective anticancer agent in in vitro and in vivo cancer models and imposed miniscule side effects. Herein we report that VO(NG) 2 is significantly cytotoxic to various cancer cell lines. Furthermore, this redox active vanadyl complex altered the redox homeostatsis of many human cancer cell lines significantly. VO(NG) 2 actuates programmed cell death in human colorectal carcinoma cells(HCT-116) through mitochondrial outer membrane permeabilization but in caspase independent manner, possibly by altering cellular redox status and by inflicting DNA damage. Thus, the present work is an attempt to provide many evidences regarding the potent and selective chemotherapeutic efficacy of the novel VO(NG) 2 . [ABSTRACT FROM AUTHOR]

In India, sucking pests including leafhoppers ( Amrasca biguttula biguttula Ishida) and whitefly ( Bemisia tabaci Gennadius) cause considerable economic damage to okra cultivation. This study reports the results of field experiments evaluating the bioefficacy, phytotoxicity, and residue dynamics of sprays of flonicamid 50 WG in okra ( Abelmoschus esculenta (L.) Moench) crops. Of three doses (50, 75, 100 g a.i ha −1 ) tested, applications at 75 g a.i ha −1 were equally effective in controlling both leafhoppers and whiteflies with a higher marketable fruit yield of okra under open field conditions. Flonicamid also reduced population of the pest by >85% when compared to untreated controls after three rounds of foliar application at an interval of 10 days. Applications of flonicamid 50 WG did not cause any phytotoxic symptoms. It was also safe to the natural enemies (spiders and rove beetles) prevailing in the okra ecosystem. Initial deposits of flonicamid in okra fruits when applied at the rate of 75 and 150 g a.i. ha −1 were dissipated with half-lives of 3.0 and 3.5 days. Recommendable pre-harvest intervals (PHI) are 16 and 20 days, respectively. The dietary exposure of the measured residues was lower than the maximum permissible intake (MPI) of 0.576 mg person −1 day −1 on all the sampling days at both the doses. These findings are useful in deciding the spray schedule of flonicamid for effective management of sucking pests in okra crop assuring food safety. [ABSTRACT FROM AUTHOR]

T-cell acute lymphoblastic leukemia (T-ALL) is an aggressive form of cancer and the therapeutic outcome for T-ALL patients remains poor. Thus innovative therapeutic strategies with less toxic drugs are of immense need. Moreover combinational effect of redox imbalance with modulated EGFR/PI3K/Akt axis in T-ALL is still elusive. To explore more effective drugs we developed and characterized 5-SMAG, Cu-5-SMAG and Cu-OBPHA complexes by different spectroscopic methods and revealed that introduction of methoxy group and copper to the previously synthesized Schiff base ligand, NG can efficiently target leukemia by sparing the normal cells and overcomes MDR in T-ALL through induction of caspase3 dependent apoptosis as assessed by MTT, Cell-cycle, Annexin-V and caspase3 activation assay. However the ligand 5-SMAG fails to exert significant cytotoxicity. Moreover introduction of copper does not increase the efficacy of the drug molecule as Cu-OBPHA fails to exert significant effect compared to Cu-5-SMAG. Moreover Cu-5-SMAG targets T-ALL cells more than Cu-OBPHA because Cu-5-SMAG generates greater extent of redox imbalance compared to Cu-OBPHA and when this redox imbalance is reduced by application of NAC and PEG-Catalase, highest abrogation of apoptosis is observed following Cu-5-SMAG treatment In addition, Cu-5-SMAG significantly down-regulates the activation and expression of EGFR1, Akt and PI3K in drug-resistant T-ALL cells. Furthermore Cu-5-SMAG significantly increases the life-span of doxorubicin resistant and sensitive Ehrlich ascites carcinoma bearing Swiss albino mice without inducing any significant systemic toxicity compared to 5-SMAG and Cu-OBPHA treatment. Therefore typical architect of Cu-5-SMAG made it a promising new anti-leukemic agent irrespective of the MDR phenotype. [ABSTRACT FROM AUTHOR]

A method was validated for the simultaneous analysis of the residues of dimethomorph, famoxadone and cymoxanil in grape and raisin matrix by ethyl acetate based extraction and liquid chromatography tandem mass spectrometric analysis. Field studies were conducted to evaluate the dissipation rate kinetics and processing factor (PF) for these pesticides during raisin making. Residue data during the drying process were best fitted to 1st + 1st order rate kinetics with half-life ranging between 8–9 days for dimethomorph, 12–13 days for famoxadone and 9–10 days for cymoxanil at single dose (SD) and double dose (DD), respectively. PF values calculated were 1.03 and 1.14 for dimethomorph, 1.95 and 2.09 for famoxadone, and 1.99 and 1.35 for cymoxanil at SD and DD, respectively. PF value >1 indicates concentration of the residues during raisin making. The residues of detected pesticides in market samples of raisins were devoid of any risk of acute toxicity related to dietary exposure. [ABSTRACT FROM AUTHOR]

Highlights: [•] Dissipation kinetics of the residues of CPPU, 6-BA, GA3 and Ethephon in grape are reported. [•] Dissipation of residues followed 1st +1st order kinetics. [•] Initial residue of GA3 was below MRL and hence no pre-harvest interval (PHI) is applicable. [•] CPPU, 6-BA and Ethephon residues dissipated with PHIs of 33.5, 12 and 32days, respectively. [Copyright &y& Elsevier]

Abstract: A single quadrupole GC–MS method was optimized for multiresidue determination of 47 pesticides in grapes with limit of quantifications of each compound in compliance with the EU-MRL requirements. Sample preparation involved extraction of 10g sample with 10ml ethyl acetate (+10g sodium sulphate) by homogenization at 15,000rpm followed by centrifugation at 3000rpm. The supernatant was cleaned by dispersive solid phase extraction with primary secondary amine and acidified with 0.1% formic acid. Residues were estimated in selected ion monitoring mode with programmable temperature vaporizer-large volume injection (8μl). All the GC and MS parameters were thoroughly optimized to achieve satisfactory linearity (R 2 >0.99) within 0.01–0.25mgkg−1 with minimum matrix interferences. Recoveries at 0.01 and 0.02mgkg−1 were within 67–120% with associated precision RSD below 19%. The method was successfully applied for analysis of the real world samples for incurred residues. [Copyright &y& Elsevier]

Abstract: Food safety aspects of buprofezin, dimethoate and imidacloprid residues in pomegranate are reported. The residue analysis involved extraction of samples (15g) with 10ml ethyl acetate, cleanup by dispersive solid phase extraction with 25mg primary secondary amine and 25mg C18 sorbents and estimation by LC–MS/MS. The limit of quantification of each analyte was 0.001mgkg−1 with recoveries within 76–109%. The residues of buprofezin and dimethoate were confined to outer rind, which degraded to below the maximum residue limit for the European Union (EU-MRL) after 10.5 and 31.5days at standard dose and 32.0 and 44.0days at double dose. Residues of imidacloprid penetrated into the albedo and membrane, although at less than the MRL in all samples even at double dose. The dietary exposure of buprofezin and imidacloprid was safe on all sampling days; whereas samples with dimethoate appeared safe after 15 and 30days of field applications at standard and double doses, respectively. [Copyright &y& Elsevier]

Abstract: An aqueous extraction method coupled with ultra performance liquid chromatography with photo diode array detection was optimised and validated for screening of 93 garlic ecotypes for allicin and other allyl thiosulphinate contents. Variability in allicin, allyl methyl thiosulphinate and allyl trans-1-propenyl thiosulphinate was observed both on fresh and dry weight basis. Bulb to bulb variation for allicin levels was less in clonal selections followed by commercial varieties, exotic line and landraces, respectively. Five ecotypes on fresh weight basis and all the ecotypes on dry weight basis had allicin contents more than the recommended pharmacological values (⩾4.5mgg−1). Cluster analysis and principal component analysis results revealed that geographical origin, breeding status and colour did not play any role in ecotype clustering. This study is useful as a base for selection of garlic ecotypes as a dependable raw material source for pharmaceutical and food processing industries. [Copyright &y& Elsevier]

Abstract: Multidrug resistance (MDR) mediated by the over expression of drug efflux protein P-glycoprotein (P-gp) is one of the major impediments to successful treatment of cancer. P-gp acts as an energy-dependent drug efflux pump and reduces the intracellular concentration of structurally unrelated drugs inside the cells. Therefore, there is an urgent need for development of new compound that are less toxic and effective against drug resistance in cancer. Preclinical studies have shown that quinoline derivatives possess anticancer activities. Here, we report the antitumor potential of quinoline derivative, 2-(2-Methyl-quinolin-4ylamino)-N-phenyl acetamide (S4). To evaluate the cytotoxic potential of S4, we used four different cell lines (Hela, HCT-116, CCRF-CEM, and CEM/ADR 5000) in vitro, and showed that S4 kills doxorubicin resistant T lymphoblastic leukemia cell, CEM/ADR 5000 in a concentration dependent manner while others remains unaffected. Moreover, S4 induces apoptosis in CEM/ADR 5000 cells through generation reactive oxygen species (ROS). This is substantiated by the fact that the antioxidant N-acetyle-cysteine (NAC) completely blocks ROS generation and, subsequently, abrogates S4 induced apoptosis. Furthermore, in vivo treatment with S4 significantly increases the life span of swiss albino mice bearing sensitive and doxorubicin resistant subline of Ehrlich ascites carcinoma. In addition, intraperitoneal application of S4 in mice does not show any systemic toxicity at concentrations that in preliminary trials in a mice Ehrlich ascites carcinoma model. Therefore, present report provides evidence that S4, a quinoline derivative, may be a promising new therapeutic agent against drug resistant cancers. [Copyright &y& Elsevier]

Abstract: A novel method for the residue analysis of wine spoilage compound 2,4,6-trichloroanisole is reported. Wine (60ml) was extracted with 2ml toluene in presence of 24g MgSO4 and 6g NaCl. Cleanup of the toluene phase by dispersive solid phase extraction with mixture of 100mg CaCl2, 25mg primary secondary amine and 50mg MgSO4 was effective in minimising co-extractives and matrix effects. Time-of-flight and tandem mass spectrometric parameters were optimised to achieve linearity over 0.25–500ngml−1 and method detection limit 0.0083ngml−1 which is well below the odour threshold of 0.04ngml−1. Recoveries at 0.04, 0.2 and 0.8ngml−1 were within 80–110% (±8%). The method was reproducible when tested for Argentinean wines with intra-laboratory Horwitz ratios being <0.20 in white and red wines at both the laboratories of India and Argentina. The method could be successfully applied for incurred wine samples. [ABSTRACT FROM AUTHOR]

The global vegetable oil market is valued at US$105.6 billion, with sunflower seed oil ranking fourth in consumption. However, recent events like the COVID-19 pandemic and regional conflicts have disrupted production and supply chains, leaving them vulnerable to fraudulent practices such as adulteration with cheaper oils and mineral oils. This review analyses the underlying causes and consequences of adulteration in the sunflower oil industry, as well as the analytical techniques utilized for its identification and mitigation. Consuming low-quality imported food due to economically motivated adulteration can adversely affect the economy and consumer health. For instance, the food poisoning epidemic caused by Spain's fake olive oil scandal severely jeopardized the country's consumer health. Thus, considering these factors, a two-tier approach is required to identify and mitigate the occurrence of fraud and any contaminants. The tier 1 rapid screening tool is a Raman spectroscopic technique coupled with chemometrics for the on-package in situ inspection, and the tier 2 confirmation tool is a chromatographic technique augmented with mass spectrometry to authenticate suspect samples identified in tier 1 screening. Incorporating Artificial Intelligence and the Internet of Things (IoT) in a two-tier approach can efficiently ensure food safety in the global supply chains. • A summary of safety and fraud challenges in sunflower oil, especially those emerging challenges arose in recent years. • A systematic review of a multidisciplinary two-tier approach to analytical tools for testing sunflower oil authenticity. • A comparison among those different type of tools in both performances and application scenarios. • Insights on data processing workflows and revealing AI's potential in non-targeted multivariate analysis. • Smart approach for food industry and regulators to ensure consumer safety with effective prevention measures. [ABSTRACT FROM AUTHOR]

This paper reports a selective and sensitive method for multiresidue determination of 119 chemical residues including pesticides and polyaromatic hydrocarbons (PAH) in high fatty fish matrix. The novel sample preparation method involved extraction of the target analytes from homogenized fish meat (5 g) in acetonitrile (15 mL, 1% acetic acid) after three-phase partitioning with hexane (2 mL) and the remaining aqueous layer. An aliquot (1.5 mL) of the acetonitrile layer was aspirated and subjected to two-stage dispersive solid phase extraction (dSPE) cleanup and the residues were finally estimated by gas chromatography mass spectrometry with selected reaction monitoring (GC–MS/MS). The co-eluted matrix components were identified on the basis of their accurate mass by GC with quadrupole time of flight MS. Addition of hexane during extraction and optimized dSPE cleanup significantly minimized the matrix effects. Recoveries at 10, 25 and 50 μg/kg were within 60–120% with associated precision, RSD < 11%. [ABSTRACT FROM AUTHOR]

This study presents the contents of α-methylenecyclopropylglycine, a potentially toxic amino acid, in the peel, pulp and seed fractions of two well-known litchi varieties, namely Shahi and China, over a span of three harvest-seasons. For analysing α-methylenecyclopropylglycine, an LC-MS/MS-based method was validated. The method-accuracies fell within 75–110 % (RSD, <15 %) at 0.1 mg/kg (LOQ) and higher levels. A comparative evaluation of the results in peel, pulp and seed at 30 days before harvest (DBH), 15-DBH, and edible-ripe stage revealed that α-methylenecyclopropylglycine content increased as the litchi seeds grew towards maturity, regardless of the cultivar. In arils, at maturity, the concentration of α-methylenecyclopropylglycine ranged from not-detected to 11.7 μg/g dry weight. The Shahi cultivar showed slightly higher α-methylenecyclopropylglycine content in comparison to China litchi. This paper presents the first known analysis of combined seasonal data on different fruit components at various growth stages for the two chosen litchi cultivars grown in India. • An LC-MS/MS method optimised for estimation of α-methylenecyclopropylglycine in litchi • MCPG was quantified in peel, seed and aril of China and Shahi litchi at 3 growth stages • MCPG in litchi aril ranged between 0 and 11.7 μg/g DW • Shahi litchi showed slightly higher MCPG content over China cultivar • Ripe arils showed higher MCPG over unripe in Shahi cultivar [ABSTRACT FROM AUTHOR]

[Display omitted] • Untargeted lipidomics analysis of loliginidae squid rings using UHPLC-Q-Orbitrap. • Chemometrics models accurately predict species identity of three loliginidae squids. • Comprehensive set of lipid biomarkers putatively identified for species discrimination. • Relative abundance of bioactive lipids of dietary significance mapped in squid species. Species mislabeling of commercial loliginidae squid can undermine important conservation efforts and prevent consumers from making informed decisions. A comprehensive lipidomic fingerprint of Uroteuthis singhalensis , Uroteuthis edulis, and Uroteuthis duvauceli rings was established using high-resolution mass spectrometry-based lipidomics and chemoinformatics analysis. The principal component analysis showed a clear separation of sample groups, with R2X and Q2 values of 0.97 and 0.85 for ESI+ and 0.96 and 0.86 for ESI-, indicating a good model fit. The optimized OPLS-DA and PLS-DA models could discriminate the species identity of validation samples with 100 % accuracy. A total of 67 and 90 lipid molecules were putatively identified as biomarkers in ESI+ and ESI-, respectively. Identified lipids, including PC(40:6), C14 sphingomyelin, PS(O-36:0), and PE(41:4), played an important role in species discrimination. For the first time, this study provides a detailed lipidomics profile of commercially important loliginidae squid and establishes a faster workflow for species authentication. [ABSTRACT FROM AUTHOR]

A novel assessment of the conservatism in the UNF-ST&DARDS decay heat calculations has been performed. UNF-ST&DARDS is used to quantify the uncredited margin in safety analysis calculations for spent nuclear fuel (SNF) storage, transportation, and disposal systems. The goal of the assembly-specific as-loaded safety analysis approach in UNF-ST&DARDS is to determine the time-dependent realistic state of the SNF systems; however, it is desirable to conservatively estimate safety analysis parameters, such as decay heat, for a given set of fuel characteristics. The primary source of conservatism in the generic UNF-ST&DARDS assembly-specific as-loaded analysis (also referred to as bounding within UNF-ST&DARDS) is the conservative assumptions of various reactor operational parameters that attempt to envelop wide spectrum of reactor operating scenarios. The assessment in this paper is necessary to demonstrate that sufficient decay heat conservatism is retained in the UNF-ST&DARDS bounding as-loaded spent fuel analysis methodology. This paper also demonstrates the time dependent impact of various parameters such as last cycle power on decay heat values. A comparison between the UNF-ST&DARDS bounding decay heat calculations and calculations performed using a detailed description of the fuel assembly operating histories, referred to as detailed calculations, was performed using recently acquired data. The data used to perform this evaluation are from one set of 3019 assemblies from a US boiling water reactor (BWR) site and one set of 2117 assemblies (952 8 × 8, and 1165 10 × 10) from a Swedish BWR reactor. Analyses of the US data involved two sets of assumptions for the bounding calculations and produced two data sets. The first analysis, in which the cycle-wise burnups were derived for the bounding calculations from the detailed data, generated the derived data set; the second, in which the assumptions associated with incorporating US nuclear fuel data survey (Form GC-859) data were included in the calculations for a subset of the same assemblies, generated the GC-859 data set. When bounding assumptions were used, the average level of conservatism (overestimation of decay heat) ranges between 9.0% and 17.7% for the derived data set, between 11.4% and 32.3% for the GC-859 data set, between 10.1% and 62.6% for the Swedish 8 × 8 fuel and between 8.3% and 44.7% for the Swedish 10 × 10 fuel. The level of conservatism and the scatter in the ratio between bounding and detailed data increase significantly for the 100- and 200-year cases for derived US and Swedish data sets. The GC-859 data set had large conservatisms in the early cooling times that initially shrank with time and then increased for the 100-year and 200-year cooling times. These results show that, while UNF-ST&DARDS can be used to calculate assembly decay heat based on assembly characteristics and operating history to identify potential significant margins to the licensing basis decay heat calculations, the decay heats calculated by UNF-ST&DARDS are still conservative compared to more detailed calculations for the range of assemblies and operating conditions assumptions evaluated in this study. [ABSTRACT FROM AUTHOR]

Highlights • A unified residue analysis method for regulatory testing of veterinary drugs & pesticides in milk was developed. • Sample preparation involved a single sub-sample followed by analysis using UFLC-MS/MS and GC–MS/MS. • The method was validated for 238 pesticides and 78 veterinary drugs. • The method provides precise and accurate analysis with significant savings in time & cost of analysis. Abstract This paper reports a unified sample preparation approach for high-throughput multi-residue analysis of veterinary drugs and pesticides in a single sub-sample of bovine milk. The sample (5 g) was deproteinized with acetonitrile before an aliquot (I) was withdrawn, and the remainder was phase-separated using MgSO 4 and NaCl. The acetonitrile layer (II) was recovered and the extracts combined, cleaned, and solvent-exchanged before the concentrations of veterinary drugs and pesticides were measured by ultra-fast liquid chromatography tandem mass spectrometry (UFLC-MS/MS). As a unique approach, extract II was analyzed simultaneously using gas chromatography tandem mass spectrometry (GC–MS/MS). Method performance for 78 drugs and 238 pesticides complied with CD 2002/657/EC and SANTE/11813/2017 guidelines, respectively, with significant savings in time and cost. Thus, it would be ideal for regulatory analysis of analytes ranging from non-polar organochlorine pesticides to polar drugs, including penicillins, quinolones, and tetracyclines. [ABSTRACT FROM AUTHOR]

Tinospora cordifolia herbal supplements have recently gained prominence due to their promising immunomodulatory and anti-viral effects against SARS-CoV-2. Mislabelling or diluting Tinospora supplements for profit may harm public health. Thus, validating the label claim of these supplements in markets is critical. This study investigated how high resolution mass spectrometry-based metabolomics and chemometrics can be used to distinguish Tinospora cordifolia from two other closely related species (T. crispa and T. sinensis). The Orthogonal Partial Least Square Discriminant Analysis (OPLS-DA) and PLS-DA based chemometric models predicted the species identity of Tinospora with 94.44% accuracy. These classification models were trained using 54 T. cordifolia , 21 T. crispa , and 21 T. sinensis samples. We identified 7 biomarkers, including corydine, malabarolide, ecdysterone, and reticuline, which discriminated Tinospora cordifolia from the two other species. The label claim of 25 commercial Tinospora samples collected from different parts of India was verified based on the relative abundance of the biomarker compounds, of which 20 were found authentic. The relative abundance of biomarkers significantly varied in the 5 suspicious market samples. This pilot study demonstrates a robust metabolomic approach for authenticating Tinospora species, which can further be used in other herbal matrices for product authentication and securing quality. [Display omitted] • HRMS-based metabolomic fingerprinting for species authentication in herbal supplements of Tinospora cordifolia. • Metabolites were identified using comprehensive custom curated accurate mass library. • Chemometric models were developed as proof of concept for authenticating Tinospora cordifolia herbal supplements. • Biomarkers were identified and their relative abundance were compared in authentic and adulterated samples. • This study could help in developing a rugged method for regulatory control of quality and authenticity of herbal supplements. [ABSTRACT FROM AUTHOR]

Higher matrix interference makes the multi-residue pesticide analysis in spices more challenging. A simple, sensitive, and robust large-scale multi-residue method was developed for the rapid analysis of 243 pesticides in cardamom matrix by gas chromatography tandem mass spectrometry (GC-MS/MS). Prehydration of cardamom in 1:4 sample:water for 30 min improved the homogeneity and extractability. QuEChERS extraction followed by cleanup with 25 mg primary secondary amine, 100 mg C 18 , and 10 mg graphitized carbon black to 1 ml supernatant was used for sample preparation. Reconstitution of final extract in ethyl acetate reduced matrix co-extract up to 60%. The method was validated according to the SANTE/11,945/2015 guidelines. The limit of quantification was ≤0.01 mg kg −1 , and the recovery was within 70.0–120.0%, with ≤20% RSD for the majority of pesticides. The method was used for screening market samples, and the detected residues were devoid of any risk of acute toxicity related to dietary exposure. [ABSTRACT FROM AUTHOR]

Tuber crops substantially contribute to the food security in the developing countries. Often, their cultivation involves unregulated applications of pesticides, leading to MRL non-compliances. Despite their rising currency in international trade, there exist scarcely any methods for pesticide residue analysis in these matrices. Therefore, we developed a multi-residue method for simultaneous analysis of a diverse range of pesticides in tuber crops, based on pressurized liquid extraction by ethyl acetate, followed by selective identification and quantification of the residues using GC–MS selected reaction monitoring. The method was evaluated for 150 pesticides. Results showed that their limits of quantification were 0.1–10 ng/g, with recoveries of 70–120%. When compared to the conventional analytical techniques, such as QuEChERS and buffered ethyl acetate extraction, this method provided superior performance in terms of precision, and recovery of the spiked and incurred residues with similar productivity. The method holds promise for commercial and regulatory residue analysis. [ABSTRACT FROM AUTHOR]

A buffered ethyl acetate extraction method was optimized and validated in raisin matrix to monitor 276 pesticides by liquid chromatography–tandem mass spectrometry (LC-MS/MS) analysis. The final method involved homogenization of raisinsalong with water 1:1 raisins: water followed by extraction using ethyl acetate (10 mL/10 g raisins homogenate in presence of 0.1 mL acetic acid, 0.5 g sodium acetate and 10 g sodium sulfate, and cleanup by dispersive solid phase extraction with primary secondary amine sorbent (25 mg/5 mL extract). 276 pesticides were estimated within 20 min of chromatographic run time by retention time dependent ‘scheduled multiple reaction monitoring’ (sMRM) by LC-MS/MS.The method was validated as per European guideline, DG-SANTE/11945/2015, at 2, 10, and 25 ng/g spiking levels where the method precision in terms of repeatability was <15% at 10 ng/g for 93.8% of the compounds. The Limit of quantification (LOQ) ranged between 0.01 and 10 ng/g with recoveries 70–120% with ≤20% RSD for 93.5% of compounds at regulatory default MRL of 10 ng/g. The matrix induced signal suppressions or enhancement were moderate (60–130% accuracy against solvent standard) for 85% compounds in white raisins and 67% compounds in black raisins. The method was successfully applied for screening of 94 market samples of raisins for the target analytes. The dietaryexposures calculated against the average concentrations detected were wellbelow the maximum permissible intake (MPI) values and the collected raisin samples were considered safe for human consumption without any acute toxicity hazard. [ABSTRACT FROM AUTHOR]

• Investigated matrix effects in pesticide residue analysis across 4 pomegranate cultivars. • Different cultivars demonstrated different matrix effects for most pesticides. • The cultivar-wise variations in GC-MS/MS were more prominent than LC-MS/MS analysis. • Extrapolative dilutions effectively reduced the cultivar-wise variations in matrix effects. • Cultivar-specific matrix-matched standards could minimize such variability in matrix effects. Matrix effect (ME) is unavoidable in multiresidue pesticide analysis, even when using highly advanced instruments, and differences in MEs can affect residue analytical accuracy due to pomegranate cultivar composition variations. However, literature to support this claim is limited. The study used GC-MS/MS and LC-MS/MS to investigate four different Indian pomegranate cultivar extracts and their MEs on multi-class pesticides. The whole fruit and arils of all cultivars were tested for 22 GC-amenable and 21 LC-amenable pesticides. Principal component analysis of the data confirmed that each cultivar had unique MEs for each pesticide. The majority of pesticides showed acute variations in recovery rates with 95% confidence, while GC-MS/MS-amenable pesticides showed more variation. Although extrapolative dilution reduced the influence of MEs on analytical accuracy, a generalized matrix-matching for all cultivars was not possible to achieve. To reduce the variability in MEs, it is recommended that a cultivar-specific matrix-matched standard should be used. [ABSTRACT FROM AUTHOR]

[Display omitted] • 5.23 g/cm3 γ-ray shields were developed by hot compacting red mud:Bi 2 O 3 (RMBi) melt. • RMBi block shows 60% attenuation of lead at 1.33 MeV. • RMBi block possess the compressive strength of ≈283 MPa, both at RT and 500 °C. • No leaching of heavy metals from the hot compacted samples. • It can reduce the usage of toxic-lead and accumulation of industrial waste. Red mud (RM) is a hazardous by-product of alumina industry, which accumulates and pollutes the environment due to inadequate technologies for large-scale utilization. This iron rich (30–60%) RM is converted into γ-ray shielding blocks as an alternative of toxic-lead and concrete. High dense γ-ray shielding blocks were fabricated by hot compacting (HC) RM (HC-RM), RM:Ba(OH) 2 ·H 2 O (HC-RMBa) and RM:Bi 2 O 3 (HC-RMBi) close to their melting point, which assist to close the pores and thereby to attain 97 to 98% of compaction. The density of HC-RM, HC-RMBa and HC-RMBi blocks are 3.34, 4.61 and 5.23 g/cm3, respectively, which is two times higher than the cold compacted (CC) ones. The linear attenuation coefficient (µ) of HC-RM, HC-RMBa and HC-RMBi blocks are 0.0209, 0.0269 and 0.0329 mm−1, respectively at 1.33 MeV (60Co). The HC-RM, HC-RMBa and HC-RMBi samples possess 38, 49 and 60% attenuation of lead at 1.33 MeV and possess the compressive strength of 34, 243 and 283 MPa, respectively. No heavy elements were found to leach out after hot compaction. The developed shields are thermally stable and found to be suitable for building radiation shielding structures in an economically viable manner than toxic-lead and concrete. [ABSTRACT FROM AUTHOR]