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Based on the excellent performances of nanocrystalline cellulose, sodium alginate, or K-carrageenan in Pb2+ adsorption, nanocrystalline cellulose/sodium alginate/K-carrageenan composite hydrogel beads were prepared to adsorb Pb(II) from aqueous solutions. The objective of this study was to demonstrate the excellent potential of the composite hydrogel beads for heavy metal ion adsorption. We successfully prepared ecofriendly Fe-modified nanocrystalline cellulose/sodium alginate/K-carrageenan composite hydrogel beads and characterized them. The structure and adsorption mechanism were investigated using scanning electron microscopy, Fourier-transform infrared spectroscopy, and X-ray photoelectron spectroscopy, and the optimal adsorption conditions were determined. The tricomponent hydrogel beads were robust and exhibited improved adsorption capacity for Pb2+ and good reusability. The adsorption results could be fitted well with a pseudo-second-order kinetic model and the Langmuir adsorption model. The maximum adsorption capacity obtained by fitting was 351.04 mg g−1. Recycling experiments revealed that the adsorption capacity of the adsorbent remained high after five cycles of reuse. [ABSTRACT FROM AUTHOR]

Surface modification of cellulose nanocrystals (CNC) is essential for improving their reactivity and adsorption capacity. Oxidation, as a conventional modification method of CNC, has strong reaction conditions, which may partially destroy the structure of CNCs. Herein, we propose a mild cellulose modification method, in which diethylenetriaminepentaacetic acid (DPTA) was grafted onto CNC with an aminosilane coupling agent. To facilitate the enrichment and recovery of adsorbents, we prepared magnetic CNC before grafting DPTA, and finally obtained magnetic carboxylic functionalized CNC (MCNC-DPTA). The effects of the reaction parameters on the adsorption process were systematically studied by transmission electron microscopy, X-ray diffraction, Vibration sample magnetometry, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. Additionally, the effects of the solution pH, the initial concentration of Pb, and the adsorption time on the adsorption properties of the materials were evaluated. Furthermore, the structure, morphology, and thermal properties of the solution were systematically studied. After 6 cycle tests, the adsorption amount of Pb(II) by MCNC-DPTA was only reduced by 7%. These results show that MCNC-DPTA is an environment-friendly adsorption material with an excellent Pb(II) removal effect. [ABSTRACT FROM AUTHOR]

The easiness-to-handle of the magnetic dispersive solid phase extraction (Mag-dSPE) procedure was developed for preconcentration of 24 steroid hormones in river water. Ethylenediamine-functionalized magnetic carbon nanotubes (EDA@Mag-CNTs) were synthesised by a simple one-pot reaction and were used as sorbent in Mag-dSPE procedure. The properties of the EDA@Mag-CNTs were characterized by transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). An ultra-fast liquid chromatography-tandem quadrupole mass spectrometry (UFLC-MS/MS) method for determination of 24 steroid hormones in river water at nanograms per liter had been developed with pretreatment of the samples by Mag-dSPE. The obtained results demonstrated the higher extraction capacity of EDA@Mag-CNT Mag-dSPE with recoveries between 82.1 and 113 %. The limits of quantification (LOQs) for the steroid hormone were between 0.020 and 1.00 ng/L. The developed method had been successfully applied to 60 river water samples, and it was confirmed that EDA@Mag-CNT Mag-dSPE was a highly effective extraction method for the steroid hormone analyses. [ABSTRACT FROM AUTHOR]

Pindone is a highly effective anticoagulant rodenticide. In this paper, an improved assay for the analysis and confirmation of pindone in human plasma has been proposed. After the samples protein precipitation with 10% ( v/v) methanol in acetonitrile and cleaning with solid-phase extraction, the separation was carried out on an IonPac AS11-HC analytical column (250 mm × 2 mm) using 20 mmol L−1 KOH containing 10% ( v/v) methanol as organic modifier by eluent generator reagent free ion chromatography. Quantification was performed by a negative electrospray ionization ion trap mass spectrometry using diphacinone as an internal standard. The transition for quantitative analysis was m/ z 229 → 172, and for qualitative analysis were m/ z 229 → 145 and m/ z 229 → 214 for pindone. The transition for quantitative analysis was m/ z 339 → 167 for IS. The limit of detection, the limit of quantification, recovery, linearity, precision, and stability were well validated. The cracking approach of characteristic fragments for pindone and IS were proposed. It was confirmed that this method could be used in clinical diagnosis and forensic toxicology analysis. [ABSTRACT FROM AUTHOR]

Analysis of diphacinone is often performed on C18 column by reserved phase liquid chromatographic methods coupled with ultraviolet detection or by ion-pair chromatography coupled with mass spectrometry. In this work, a sensitive and selective method using eluent generator reagent free ion chromatography coupled with electrospray ionization ion trap mass spectrometric detection for the quantification of diphacinone in animal livers has been developed. Samples were extracted with 10% ( v/v) methanol in acetonitrile after spiking with warfarin (internal standard, IS) and cleaned by solid-phase extraction. The analytes were separated on an IonPac AS11 analytical column (250 mm × 4.0 mm) using 30.0 mmol L−1 KOH (achieved by a KOH eluent generator) containing 10% ( v/v) methanol as organic modifier at a flow rate of 1.0 mL min−1. Detection was performed by negative electrospray ionization and ion trap tandem mass spectrometry in multiple reaction monitoring mode with a transition of m/z 339 → 167 for diphacinone, and 307 → 161 for IS, respectively. The calibration curve was linear ( r 2 = 0.993) in the concentration range of 1.0–200.0 ng mL−1 with a lower limit of quantification of 0.3 ng g−1 in animal livers. Intra- and inter-day relative standard deviations (RSDs) were less than 8.7 and 12.5%, respectively. Recoveries of diphacinone ranged from 81.2 to 89.5%. It was confirmed that this method could be used in clinical diagnosis or forensic toxicology. [ABSTRACT FROM AUTHOR]

In this study, the development and validation of an analytical method for triptolide in whole blood using high-performance liquid chromatography coupled with atmospheric-pressure chemical ionization ion trap tandem mass spectrometry (LC–APCI-IT-MS-MS) is reported. This is the first report of the systematic development and validation of an LC–MS-MS method for the quantitation of triptolide in human whole blood using prednisolone as an internal standard (IS). Prior to LC–MS-MS analysis, liquid–liquid extraction with ethyl acetate was used to isolate them from the biological matrix. Validation parameters such as specificity/selectivity, limit of quantitation (LOQ), linearity, precision, accuracy and stability are evaluated for this method. The calibration curve was linear ( r 2 = 0.9973) in the concentration range of 0.5–100.0 ng mL−1 in human whole blood with a lower limit of quantitation of 0.5 ng mL−1. Intra- and inter-day relative standard deviations (RSDs) were less than 8.6 and 11.7%, respectively. Extraction recoveries of triptolide ranged from 81.5 to 88.1%. This assay can be used to determine trace triptolide in human whole blood. [ABSTRACT FROM AUTHOR]

A rapid and sensitive method has been developed and validated to determine 6-benzyladenine (6-BA) residues in bean sprout using high-performance liquid chromatography coupled with electrospray ionization ion trap tandem mass spectrometry. Liquid–liquid extraction, using acidified methanol, was used to isolate 6-BA from the sample matrix. The separation was carried out on a Zorbax SB C18 column (150 mm × 4.6 mm i.d., 5 μm) with 0.1% acetic acid/methanol (25:75 v/ v) as mobile phase in isocratic mode. The quantitation of 6-BA was based on fragmentation of the molecular ion at m/ z 226.1 to a product ion at m/ z 91.1. In addition, the recoveries of three extraction solvents by ultrasound extraction and conventional extraction method were compared, and it was found that acidified methanol as the extraction solvent was the best. The calibration curve was linear ( r 2 > 0.997) in the concentration range of 0.04–10.0 ng mL−1 with a lower limit of quantification of 0.5 ng g−1 for 6-BA in bean sprout. Intra-day and inter-day relative standard deviations (RSDs) were less than 7.1 and 9.8%. Recoveries of 6-BA were between 85.0 and 88.5%. This assay has been successfully applied to the determination of trace 6-BA residues in bean sprout and monitoring the market in Ningbo, China. [ABSTRACT FROM AUTHOR]

A novel method using liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry in the negative selected ion monitoring mode has been developed and validated for rapid simultaneous determination of triptolide and tripdiolide in the extract of Tripterygium wilfordii Hook. f. The molecular ions m/z [M–H]− 359 and 375 were selected for the quantification in selected ion monitoring mode for triptolide and tripdiolide. Standard calibration curve was linear over the concentration range of 0.12–24 and 0.15–30 μg mL−1 for triptolide and tripdiolide. The relative standard deviations of intra- and inter-day were in the range of 4.7–9.9 and 8.9–12.6%. The average recoveries were between 96.4 and 104.6%. The limits of quantitation were 2.0 × 10−3 and 2.5 × 10−3 μg mL−1 for triptolide and tripdiolide. [ABSTRACT FROM AUTHOR]