Microbial-based metabolites associated with degradation of imidacloprid and its impact on stress-responsive proteins.

Imidacloprid (IMD), a neonicotinoid insecticide, is intensively used in agricultural fields for effective protection against aphids, cane beetles, thrips, stink bugs, locusts, etc., is causing serious environmental concerns. In recent years, seed treatment with Imidacloprid is being practiced mainly to prevent sucking insect pests. In India, due to the increase in application of this insecticide residue has been proven to have an impact on the quality of soil and water. In view of this, the current investigation is focussed on sustainable approach to minimize the residual effect of IMD in agricultural fields. The present study reveals a most promising imidacloprid resistant bacterium Lysinibacillus fusiformis IMD-Bio5 strain isolated from insecticide-contaminated soil. The isolated bacterial strain upon tested for its biodegradation potential on mineral salt medium (MSM) showed a significant survival growth at 150 g/L of IMD achieved after 3 days, whereas immobilized cells on MSM amended with 200 g/L of IMD as the sole carbon source provided degradation of 188 and 180 g/L of IMD in silica beads and sponge matrices, respectively. The liquid chromatography mass spectrometry was performed to test the metabolite responsive for IMD biodegradation potential of L. fusiformis IMD-Bio5 which showed the induced activity of the metabolite 6-Chloronicotinic acid. Furthermore, as compared to the untreated control, the Lysinibacillus fusiformis IMD-Bio5 protein profile revealed a range of patterns showing the expression of stress enzymes. Thus, results provided a most effective bacterium enabling the removal of IMD-like hazardous contaminants from the environment, which contributes to better agricultural production and soil quality, while long-term environmental advantages are restored.

ZIF-8 encapsulated-enzymes integrated nanozyme cascade biocatalysis platform for the colorimetric sensing of glucose and lactose in milk.

Cascade biocatalytic reactions have a wide range of applications, especially in the filed of food analysis. Herein, a multi-enzyme composite (ZGGPC) was prepared by in-situ synthesis of Zeolite imidazole framework-8 (ZIF-8) on Prussian blue (PB) modified carbon cloth (CC). The composite encapsulated both glucose oxidase and ß-galactosidase simultaneously during the synthesis process. CC and ZIF-8 showed high loading capacity for PB and natural enzymes, respectively. And ZIF-8 also displayed excellent tolerance in protecting enzyme activity under extreme conditions. Based on the cascade biocatalysis, ZGGPC was used to detect glucose and lactose by colorimetric method with detection limits of 1.2 µM and 1.7 mM, respectively. Benefiting from the merits of low cost, easy preparation, and good stability, the sensing system was used to successfully determine glucose and lactose in different milk samples. The present cascade biocatalysis system is hopeful to develop simple and efficient sensing platforms for food analysis.

The simultaneous degradation of prochloraz and tebuconazole in water with monitoring their degradation products using liquid chromatography-tandem mass spectrometry.

Prochloraz and tebuconazole are well-known fungicides for broad applications, including medical, industrial, and agricultural. They are frequently used simultaneously which increases the probability of their co-existing in various water sources. In this study, the analysis of PCZ or TBZ in water was performed by a direct analysis using the liquid chromatography-tandem mass spectrometry technique (LC-MS/MS). The optimized method was fully validated according to the European guidelines, SANTE/11312/2021. The complete degradation of these fungicides (each of 2 mg/L) in their single presence in the water was accomplished just after 15 min using 4.2 mM persulfate at 50 °C, while a lower concentration of persulfate (1.4 mM) leads to a degradation of prochloraz and tebuconazole, in their single existence in water, at percentages of 97 % and 98 %, respectively, after 30 min at 50 °C. On the other hand, it takes a complete hour to degrade a mixture of prochloraz and tebuconazole at percentages of 99 % and 94 %, respectively, using 1.4 mM persulfate at 50 °C. Degradation products (DPds) of prochloraz and tebuconazole, either in their single or simultaneous existing in water, were also identified and monitored during the whole degradation process by LC-MS/MS using at least two mass transitions for each DPd at both positive and negative ionization modes. It was elucidated that the persulfate degradation of prochloraz was conducted by the cleavage of the imidazole ring and the subsequent formation of a trichlorophenol, while persulfate degradation of tebuconazole was mainly accomplished by the formation of a hydroxyl structure, cleavage of the tert-butyl chain, and the subsequent formation of a ketone structure. Furthermore, a new DPd of tebuconazole (m/z = 263 Da) with a diketone structure was identified and confirmed.

Evaluation of imazalil dissipation/migration in postharvest papaya using low-temperature partition extraction and GC-MS analysis.

Methods involving solid-liquid extraction with low-temperature partition and analysis by gas chromatography coupled to mass spectrometry (GC-MS) were validated to investigate the dissipation/migration of residues of the postharvest fungicide imazalil in papaya skin, pulp, and seeds. The fruits were stored for 23 days (14 °C). Every two days, fruits from the control group and those treated with imazalil had their skin, outer pulp, inner pulp, and seeds separated and then analyzed by GC-MS. After the 23rd day, about 70% of the imazalil had dissipated. Most of the remaining residue was found in the skin; however, the small amount migrating into the pulp was above the maximum residue levels allowed by the regulatory agencies. Imazalil residue was also detected in seeds at concentrations lower than the LOQ (0.025 mg kg-1). Mass loss was the only quality parameter that showed a significant difference between the fruits of the control and study groups.

Trace determination of imidacloprid and its major metabolites in wheat-soil system.

Trace analysis method is a reliable basis for studying the translocation and metabolism of imidacloprid used as an insecticide in wheat, and it clarifies whether biologically active metabolites including residual imidacloprid, have long-lasting insecticidal potency against wheat aphids under seed treatment during the entire growth period. In this study, a highly sensitive analytical method was established to determine the residues of imidacloprid and its six metabolites (5-hydroxy imidacloprid, imidacloprid olefin, imidacloprid guanidine, imidacloprid urea, 6-chloronicotinic acid, and imidacloprid nitrosimine) in wheat-soil systems, such as in wheat leaves, wheat ears, wheat grains, roots, and soil. All the compounds were extracted using an ACN:water (8:2, v/v) mixture and purified by dispersive solid-phase extraction. The average recoveries ranged from 74.4% to 109.5% for all matrices, with intra- and inter-day variations of less than 14.9%. The limit of quantitation was in the range of 0.001-0.005 mg/kg. The method is demonstrated to be sensitive and accurate for monitoring imidacloprid and its metabolites at trace levels during the entire growth period under field conditions.

A sensitive and rapid bioanalytical method for the quantitative determination of luliconazole in rabbit eye tissues using UPLC-MS/MS assay.

Luliconazole (LCZ) is a novel antifungal imidazole with broad-spectrum and high susceptibility of Aspergillus and Fusarium are the dominant species of fungal keratitis, may potentially be a new medical treatment option for ocular fungal infection. To evaluate LCZ distribution in ocular tissues after topical application for the development of ophthalmic delivery system, it is important to have a bioanalytical method for measuring the drug concentrations in different ocular tissues and aqueous humor (AH). A selective and sensitive ultrahigh performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) method was developed for the quantification of LCZ in rabbit ocular tissues, including conjunctiva, cornea, AH, iris, lens, vitreous humor (VH), retinal choroid and sclera, using lanoconazole as internal standard (IS). Chromatographic separation was achieved on a Xterra MS, C18 column (2.1 × 50 mm, 3.5 µm) using mobile phase with formic acid solution (0.2%, v/v): acetonitrile (50:50, v/v) at a flow rate of 0.2 ml/min, and the run time was 2.5 min. Detection was performed using the transitions 354.1 → 150.3 m/z for LCZ and 320.1 → 150.3 m/z for IS by positive ion electrospray ionization in multiple reaction monitoring (MRM) mode. Method validation was conducted in accordance with U.S. Food and Drug Administration's regulatory guidelines for bioanalytical method validation. The calibration curves were linear over the concentration range from 2.80 ng/ml to 2038 ng/ml for conjunctiva, cornea and sclera, 2.09 ng/ml to 1019 ng/ml for AH, 2.09 ng/ml to 509.5 ng/ml for iris, 2.09 ng/ml to 203.8 ng/ml for retinal choroid and VH, 2.04 ng/ml to 101.9 ng/ml for lens, with all the squared correlation coefficients (r2) more than 0.99. The accuracy of the method was within the acceptable limit of 89.34%∼112.78% at the lower limit of quantification and other concentrations, Inter-day and intra-day precision values, expressed in terms of RSD (%), in all tissues were within 15% at all concentrations. The mean recoveries of LCZ in rabbit ocular tissues was 84.85%∼100.52%. No interference was found due to matrix components. Luliconazole was stable during the stability studies, including autosampler stability, benchtop stability, freeze/thaw stability and long-term stability. The method was successfully applied to the ocular pharmacokinetic and tissues distribution studies of LCZ in rabbit after topical administration of LCZ ophthalmic drug delivery system.

Determination of Cyazofamid and Its Metabolite in Oily Agricultural Products with HPLC-MS/MS.

A high-performance liquid chromatography-tandem mass spectrometry method was developed for the determination of cyazofamid and its major metabolite 4-Chloro-5-(4-tolyl)-1H-imidazole-2-carbonitrile (CCIM) in oily samples. Samples were extracted with acetonitrile, which contained 1% acetic acid and cleaned-up with C18 and Florisil absorbents. Recoveries ranged from 75.91% to 109.85% with coefficients of variation from 5.14% to 10.69%. The limits of detection (LODs) and the limits of quantification (LOQs) were >0.0020 mg kg-1 and ≤0.0040 mg·kg-1, respectively, which were smaller than maximum residue levels established by Australia for oily samples. The proposed fragmentation pathway of cyazofamid and CCIM were discussed.

HPLC Fluorescence Method for Eugenols in Basil Products Derivatized with DIBI.

Eugenols (Eugs) such as eugenol (Eug), methyleugenol (MeEug), and linalool (Lin) in basil product are the main bioactive components of basil products and have a terminal double-bond. A sensitive HPLC-fluorescence method for Eugs derivatized with 4-(4,5-diphenyl-1H-imidazol-2-yl)iodobenzene (DIBI) was developed. Good separation of DIB-Eugs was achieved within 20 min on an Atlantis T3 column (50 × 2.1 mm i.d., 3 µm) with a mobile phase of methanol-water. The calibration curves obtained with Eug standards showed good linearities in the range of 0.1-50 µM (r ≥ 0.999). The limits of detection at a signal-to-noise ratio (S/N) = 3 for Eug, MeEug, and Lin were 1.0, 6.0, and 4.8 nM, respectively. The limits of quantitation (S/N = 10) of the Eugs were lower than 19.9 nM. The accuracies for the Eugs were within 96.8-104.6%. The intra- and inter-day precisions as relative standard deviations for the Eugs were less than 1.2 and 9.6% (n = 3). The recoveries of Eug, MeEug, and Lin were 99.0 ± 0.1, 98.0 ± 0.2, and 96.0 ± 0.4% (n = 3), respectively. The DIB-Eugs were confirmed to be stable for 2 h (>90%) at room temperature and 24 h (>95%) at 4 °C. These parameters of the proposed method were useful for the simultaneous determination of Eugs in basil products. Therefore, the developed method may be a powerful tool for the quality evaluation of dried commercially available basil products.

A novel stability-indicating HPLC method for the determination of enantiomeric purity of eluxadoline drug: Amylose tris(3,5-dichlorophenyl carbamate) stationary phase.

A simple and sensitive stability-indicating chiral HPLC method has been developed and validated per International Conference on Harmonization guidelines for the determination of enantiomeric purity of eluxadoline (Exdl). The impact of different mobile phase compositions and chiral stationary phases on the separation of Exdl enantiomer along with process- and degradation-related impurities has been studied. Homogeneity of Exdl and stable results of Exdl enantiomer in all degraded samples reveal the fact that the proposed method was specific (stability indicating). Amylose tris(3,5-dichlorophenyl carbamate) stationary phase column Chiralpak IE-3 (150 × 4.6 mm, 3 µm) provided better resolution with polar organic solvents than cellulose derivative, crown ether, and zwitterion stationary phases and nonpolar solvents. The mobile phase consisted of acetonitrile, tetrahydrofuran, methanol, butylamine, and acetic acid in the ratio of 500:500:20:2:1.5 (v/v/v/v/v). Isocratic elution was performed at a flow rate of 1.0 mL/min, column temperature of 35°C, injection volume of 10 µL, and UV detection of 240 nm. The United States Pharmacopeia (USP) resolution of the Exdl enantiomer was found to be more than 4.0 within a 65-min run time. Exdl enantiomer detector response linearity over the concentration range of 0.859-4.524 µg/mL was found to be R2  = 0.9985. The limit of detection, limit of quantification, and average percentage recovery values were established as 0.283 µg/mL, 0.859 µg/mL, and 96.0, respectively.

Analysis of pesticide residues by a support vector machine combined with fluorescence spectroscopy.

Pesticide residues enter a lake through the water cycle, causing harm to the water environment and human health. It is necessary to select highly sensitive fluorescence spectroscopy to detect pesticides (bifenthrin, prochloraz, and cyromazine), and a support vector machine (SVM) is used to analyze the concentration of pesticides. In addition, this paper adopts K-fold cross validation and a grid search to optimize the SVM algorithm. The performance evaluation index and running time prove the reliability of the results of this experiment. They show that fluorescence spectroscopy combined with SVM is efficient in predicting pesticide residue content.

RP-HPLC method development and validation for quantification of daclatasvir dihydrochloride and its application to pharmaceutical dosage form.

Daclatasvir dihydrochloride is an antiviral drug used in the treatment of Hepatitis C and for its estimation in drug product, no Pharmacopeial method is available. Therefore, a simple, rapid, precise and accurate isocratic RP-HPLC method was developed and validated for quantification of daclatasvir dihydrochloride in pharmaceutical dosage form. The quantification was carried out using Hypersil ODS - C18 Column (250mm, 4.6mm, 5µm), Shimadzu LC-2030 Prominence-I Series. The mobile phase composed of phosphate buffer (pH 3.5, adjusted with ortho phosphoric acid) and acetonitrile (60:40 v/v). The flow rate was 1.0ml/min with UV detection at 308 nm. The validation of developed method was conducted for specificity, linearity, accuracy, precision, LOD and LOQ. A linearity was established in the concentration range of 0.5-150% with coefficient of correlation 0.9993. The limit of detection (LOD) was 0.005µg/ml and the limit of quantification (LOQ) was 0.01µg/ml. The method was successfully applied to the assay and in-vitro dissolution studies of daclatasvir dihydrochloride in tablet dosage form. It can be concluded that this method can be very helpful in the quality control estimation of daclatasvir dihydrochloride in different pharmaceutical products intended for hepatitis C infections.

Mechanical stimulus-evoked signal transduction between keratinocytes and sensory neurons via extracellular ATP.

The skin is exposed to various external stimuli. Keratinocytes, which are the main cell type in the epidermis, interact with peripheral sensory neurons and modulate neuronal activity. Recent studies have revealed that keratinocytes play crucial roles in nociception, and that ATP is one of the main mediators of signal transduction from keratinocytes to sensory neurons. However, no quantitative cellular level analyses of ATP-mediated information flow from keratinocytes to sensory dorsal root ganglion (DRG) neurons have been conducted. In this study, we performed simultaneous imaging of cell surface ATP and intracellular Ca2+ signals using both iATPSnFR, a genetically encoded ATP probe localized to the outside of the cell membrane, and the Ca2+ probe, Fura-red. Upon mechanical stimulation of the keratinocyte with a glass needle, an increase in Ca2+ and ATP release were observed around the stimulated area, and these phenomena were positively correlated. In cultured DRG neurons and keratinocytes neighboring the stimulated keratinocyte, increased intracellular Ca2+ concentration and levels of cell surface ATP on the side closer to the stimulated cell were detected. The ratio of Ca2+ response to input ATP signal was significantly larger in DRG neurons than in keratinocytes. We found that DRG neurons were more sensitive to ATP than keratinocytes, and therefore, only DRG neurons responded to ATP at 1 µM or lower concentrations when in co-culture with keratinocytes. Moreover, signals caused by moderate mechanical stimulation of keratinocytes were transmitted predominantly to DRG neurons. These findings would be important in the further determination of the detailed mechanism of nociception in the epidermis.

Cutting agents in cocaine: A temporal study of the period 2015-2017 in the Northern Region of Colombia.

Cocaine is a naturally occurring psychostimulant drug available worldwide. Drug trafficking networks adulterate pure cocaine with cutting agents to increase their earnings. This study presents a descriptive statistical analysis of the cutting agents found in 2118 cocaine samples that were seized in the Northern Region of Colombia (in the period 2015-2017). The data used in this study was drawn from the GC-MS analytical reports of the National Institute of Legal Medicine and Forensic Sciences -Colombia, Northern Region. Results showed diverse cutting agents in seized cocaine samples, from which the most commonly used are caffeine, phenacetin, lidocaine, imidazole and levamisole. In addition, cocaine samples showed different mixtures of the above cutting agents, predominantly caffeine/phenacetin and caffeine/lidocaine/phenacetin mixtures.

Stability-indicating UPLC, TLC-densitometric and UV-spectrophotometric methods for alcaftadine determination.

Three sensitive and precise stability-indicating methods were developed for the determination of alcaftadine in the presence of its degradation products. Efficient separation was achieved using UPLC-UV-MS method by gradient elution with a mobile phase of 0.1% aqueous formic acid (A) and 0.1% formic acid in acetonitrile (B) over concentration range of 0.10-1.00 µg mL-1. The accuracy was 100.89% ± 0.74 and 99.73% ± 0.78 for UV and MS detection, respectively. A TLC-densitometric method was adopted to separate of the intact drug from its degradation products. Methanol: chloroform: glacial acetic acid (5:4:0.1, v/v/v) was the developing system, detection wavelength was set to 282 nm. Rf values were 0.35, 0.65 and 0.88 for alcaftadine, its acidic and oxidative degradants, respectively. The linearity range was 2.00-27.00 µg/band with mean accuracy of 100.58% ± 0.86. The proposed TLC-densitometric method was utilized for the study of degradation rates of alcaftadine. Finally, a simple UV-spectrophotometric method where an induced dual wavelength was implemented, the method showed a linearity range of 2.00-27.00 µg mL-1 with mean recovery of 100.15% ± 0.70. The proposed methods were successful for quantitation of alcaftadine in ophthalmic solution and in plasma samples. The obtained results were in accordance with those obtained by previously reported methods.

L-Histidine-DNA interaction: a strategy for the improvement of the fluorescence signal of poly(adenine) DNA-templated gold nanoclusters.

An interesting phenomenon is described that the fluorescence signal of poly(adenine) (A) DNA-templated gold nanoclusters (AuNCs) is greatly improved in the presence of L-histidine by means of L-histidine-DNA interaction. The modified nanoclusters display strong fluorescence emission with excitation/emission maxima at 290/475 nm. The fluorescence quantum yield (QY) is improved from 1.9 to 6.5%. Fluorescence enhancement is mainly ascribed to the L-histidine-DNA interaction leading to conformational changes of the poly(A) DNA template, which offer a better microenvironment to protect AuNCs. The assay enables L-histidine to be determined with good sensitivity and a linear response that covers the 1 to 50 nM L-histidine concentration range with a 0.3 nM limit of detection. The proposed method has been applied to the determination of imidazole-containing drugs in pharmaceutical samples. A turn-on fluorescent method has been designed for the sensitive detection of L-histidine as well as imidazole-containing drugs on the basis of the L-histidine-DNA interaction.

Chromatographic separation of the interconverting enantiomers of imidazo- and triazole-fused benzodiazepines.

The toolbox of medicinal chemists includes the 1,4-benzodiazepine scaffold as a "privileged scaffold" in drug discovery. Several biologically active small molecules containing a 1,4-benzodiazepine scaffold have been approved by the FDA for the treatment of various diseases, with most of them being used for their psychotropic effects. The therapeutic potential of 1,4-benzodiazepines has stimulated the interest of synthetic chemists in developing new synthetic strategies to a range of substituted analogues for biological evaluation. A structural variation of the classical benzodiazepine skeleton is observed e.g. in alprazolam, midazolam, and related benzodiazepines, which contain a 1,2,4-triazole or an imidazole ring fused to the benzodiazepine core. Irrespective of the presence of the fused heterocyclic ring, the seven-membered diazepine ring is far from planar, and its shape resembles a twist chair. Then, the unsymmetrical substitution pattern around the seven membered cycle renders these molecules chiral, as they lack any reflection-type symmetry element. However, chirality of this molecules is labile at room temperature, becausea simple ring flipping process converts one enantiomer into the other, and 1,4-benzodiazepines exist as a mixture of rapidly interconverting conformational enantiomers in solution at or near room temperature. Physical separation of the interconverting enantiomers of diazepam and of other related 1,4-benzodiazepin-2-ones can be accomplished by low temperature HPLC on chiral stationary phases (CSPs). If the HPLC column is cooled down to temperatures where the interconversion rate is sufficiently low, compared to the chromatographic separation rate, distinct separated peaks can be observed, provided the CSP is sufficiently enantioselctive. The apparent rate constants for the on-column enantiomerization and the corresponding free energy activation barriers were obtained by simulation of exchange-deformed HPLC profiles using a computer program based on the stochastic model. Here we report on the dynamic HPLC investigations carried out on a set of fused imidazo and triazolo-benzodiazepines (alprazolam, midazolam, triazolam and estazolam) The experimental dynamic chromatograms and the corresponding interconversion barriers reported in this paper show that the third fused heterocyclic ring increase the energy barrier by 2 kcal/mol.

An integrated method for monitoring thermal processing temperature of pork based on Q-Exactive mass spectrometry and chemometrics.

Meat heating endpoint temperature (EPT) is an important indicator to ensure the safety of cooked meat. Accurately determining the EPT of cooked meat and ready-to-eat meat products is an important strategy to ensure food safety. In this study, a comprehensive metabolic method based on UPLC-Q Exactive and chemometrics was developed to study the metabolites differences among pork roasted at different temperatures in order to select markers indicating EPT and discover new toxic heat-induced compounds. A two-step extraction method was applied to avoid the loss of metabolite information caused by sample preparation. Using chemometrics, the five compounds of creatine, creatinine, 2-amino-1-methyl-6-phenylimidazo (4,5-b) pyridine (PhIP), 2-methyl-6-amino-5-hydroxymethylpyrimidine (TMP) and compound with the m/z of 114.04316 were selected as markers, and four of them were further confirmed by chemical standards. It is worth noting that TMP was discovered in roasted pork for the first time. In addition, targeting studies aimed at quantifying the selected markers were conducted at different thermal processing temperatures. From the quantification results, it can be concluded that the heat temperature not exceed 180 °C is recommended to reduce the content of toxic compounds. This study has proved that the integration of UPLC-Q Exactive and chemometrics could provide an efficient method for the study of markers related to thermal process and new toxic heat-induced compounds.

LC and NMR Studies for Identification and Characterization of Degradation Byproducts of Olmesartan Acid, Elucidation of Their Degradation Pathway and Ecotoxicity Assessment.

The discovery of various sartans, which are among the most used antihypertensive drugs in the world, is increasingly frequent not only in wastewater but also in surface water and, in some cases, even in drinking or groundwater. In this paper, the degradation pathway of olmesartan acid, one of the most used sartans, was investigated by simulating the chlorination process normally used in a wastewater treatment plant to reduce similar emerging pollutants. The structures of nine isolated degradation byproducts (DPs), eight of which were isolated for the first time, were separated via chromatography column and HPLC methods, identified by combining nuclear magnetic resonance and mass spectrometry, and justified by a proposed mechanism of formation beginning from the parent drug. Ecotoxicity tests on olmesartan acid and its nine DPs showed that 50% of the investigated byproducts inhibited the target species Aliivibrio fischeri and Raphidocelis subcapitata, causing functional decreases of 18% and 53%, respectively.

Separation of tetrahydrozoline enantiomers in capillary electrophoresis with cyclodextrin-type chiral selectors and investigation of chiral recognition mechanisms.

The recognition power and affinity pattern of various cyclodextrins (CD) towards the enantiomers of tetrahydrozoline (THZ) were studied using capillary electrophoresis (CE). As expected, affinity of THZ enantiomers and selectivity of recognition towards CD derivatives was strongly dependent on the cavity size and substituent type and pattern on the CD rims. Not only were the affinity strength and selectivity of recognition affected by the size of the cavity and chemistry of the CDs but also the affinity pattern. Another interesting example of opposite affinity pattern of enantiomers towards α- and ß-CD was observed here. In addition, opposite affinity pattern of THZ enantiomers was seen towards ß-CD and its acetylated derivatives, while methylation of ß-CD did not affect the affinity pattern of THZ enantiomers. In order to get more information about structural mechanisms of the multivariate dependences mentioned above, rotating frame Overhauser enhancement spectroscopy (ROESY) and computation techniques were used. Significant differences between the structure of THZ complexes with different CDs with both methods were encountered. Good correlations between experimentally determined and computed structure of complexes, as well as between computed complex stabilities and enantiomer migration order (EMO) in CE were observed.

Cucurbit[7]uril as a matrix solid-phase dispersion for the extraction of quaternary ammonium pesticides from vegetables and their determination using HPLC-UV.

Cucurbit[7]uril (Q[7]) was first used as a dispersant sorbent material in a matrix solid-phase dispersion for the simultaneous extraction of four quaternary ammonium pesticides from vegetables before analysis using high-performance liquid chromatography with UV detection. Q[7] exhibited a better selectivity and adsorption capability for these compounds, which is due to its ability to bind selectively organic molecules into its hydrophobic cavity and to form stable host-guest inclusion complexes. Various parameters affecting the extraction were investigated and optimized, such as sorbent/sample mass ratio, grinding time, rinsing and eluting conditions. Under optimized conditions, the proposed method exhibited a linear response in the concentration range of 1-100 µg·kg-1, satisfactory recoveries for eight types of vegetable samples (>70%), and high repeatability (RSD < 9.0%). The limits of quantification were between 0.43 µg·kg-1 and 0.99 µg·kg-1, which is nearly 50 times lower than the maximum residue limits established by the European Council.