ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY
·
2020
·
IF 4.872
Yue Su,Weijun Wang,Jiye Hu,Xiaolu Liu
The dissipation and residues of tembotrione in corn field application were investigated using liquid chromatography tandem mass spectrometry (LC-MS/MS) method. The average recoveries of tembotrione in maize, corncob, and straw were in the ranges of 98–107% with relative standard deviations (RSDs ≤9.3%), respectively. The recoveries of M5 was in the ranges of 90–108% in all three matrices of maize, with RSDs were 3.3–12.8%. The LODs for tembotrione and M5 in maize were 0.85 μg/L and 1.0 μg/L, 0.84 μg/L and 0.43 μg/L in corncob, 0.94 μg/L and 1.5 μg/L in straw, respectively. The LOQs of the method in maize grain, corncob and straw were 0.01, 0.01 and 0.05 mg/kg for both analytes, respectively. The dissipation of tembotrione in straw was in compliance with the first-order dynamic equation, with half-lives of 1.18–1.23 days at Beijing and Heilongjiang. Total residue of tembotrione in maize grain and corncob matrix were both below 0.02 mg/kg, lower than the max residue limit (MRL) recommended by european food safety authority (EFSA). Risk quotients (RQs) of this pesticide was assessed via comparing national estimated daily intake with acceptable daily intake . The dietary intake risk of tembotrione residue in maize was very low for all groups of Chinese residents. These data could provide scientific data and strategies and facilitate Chinese government to establish the MRLs of tembotrione.
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Analytical Methods
·
2021
·Vol. 13
·期 37
·4320-4327
·
IF 2.896
Ying Zhang,Yuhan Ning,Wanliang Liao,Weiping Wang,Ai-Jun Wang
In this work, COF-LZU1@PEI@Fe3O4 was synthesized by immobilization of COF-LZU1 onto the surface of polyethyleneimine-functionalized Fe3O4 nanoparticles (PEI@Fe3O4) and employed as an adsorbent for magnetic dispersive micro-solid phase extraction of tetracyclines (TCs). COF-LZU1@PEI@Fe3O4 was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction and nitrogen adsorption–desorption isotherms analysis. The optimal extraction and desorption conditions were as follows: 15.00 mL sample solution (pH 7.0) extracted with 5.0 mg of adsorbent for 30 min at 30 °C, and then desorbed with 1.50 mL methanol/acetonitrile/0.02 mol L−1 oxalic acid solution (v/v, 1 : 2 : 7). Good linearities were obtained between the peak area and TC concentration ranging from 5–500 μg L−1 with correlation coefficients (R2) higher than 0.9992 and limits of detection lower than 0.51 μg L−1. The relative standard deviations (RSDs) of intra-day and inter-day were less than 5.7% and 7.4%, respectively. The developed method was successfully applied to the determination of TCs in environmental water samples with recoveries in the range of 87.0–113.8% and RSDs less than 5.1%, suggesting great potential of COF-LZU1@PEI@Fe3O4 for efficient extraction and analysis of trace TCs in water samples.
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MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Ming-Yue Dong,Hai-Long Wu,Wan-Jun Long,Tong Wang,Ru-Qin Yu
Edible colorants, as an essential external condition of food products, can increase people’s appetite. Some businesses have used some cheap and illegal dyes instead of edible colorants to gain benefits. It not only deceives consumers, but also seriously endangers their health. In this work, two chemometric algorithms assisted high-performance liquid chromatography with diode array detection (HPLC-DAD) were proposed for screening and quantifying twelve azo dyes illegally added into different food products. All analytes were successfully eluted within 6.5 min. With the aid of the prominent “second-order advantage” of the chemometric algorithms, the overlapping peaks and unknown interferences were solved. The spiked average recoveries obtained by alternating trilinear decomposition (ATLD) and multivariate curve resolution-alternating least squares (MCR-ALS) were 82.8–111.5% with standard deviation (SD) less than 6.5% and 78.7–122.6% with SD less than 18.7%, respectively. The limits of detection were 0.01–2.56 mg kg −1 and 0.01–2.95 mg kg −1 , respectively. The results indicated that two algorithms had practical value for the simultaneous and rapid screening and determination of azo dyes in food products. Compared with other methods based on HPLC, the proposed method could flexibly handle different interferences, and had the advantages of high efficiency, simple operation and being environmentally friendly.
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RSC Advances
·
2021
·Vol. 11
·期 48
·30102-30108
·
IF 3.361
Setareh Rostami-Javanroudi,Masoud Moradi,Kiomars Sharafi,Nazir Fattahi
In the present research, several novel and natural hydrophobic deep eutectic solvents (DESs) were prepared using methyltrioctylammonium chloride (MTOAC) as the hydrogen bond acceptor (HBA) and different types of straight chain alcohols as hydrogen bond donors (HBDs). One of the DESs composed of MTOAC and n-butanol was advantageously used to develop a vortex-assisted liquid phase microextraction (VALPME) method combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) for the determination of common acaricides in fruit juice samples. Several important parameters influencing extraction efficiency were investigated and optimized, including the type and volume of DES, sample solution pH, effect of salt addition and, extraction and vortex time. Under optimal experimental conditions, the method showed good linearity with the correlation coefficients (R2) of 0.9986–0.9991 in the linear range of 2–300 μg L−1, low limits of detection of 0.5–1 μg L−1 and acceptable extraction recoveries in the range of 85–93%. The proposed method was successfully applied for the extraction and preconcentration of trace acaricides in real fruit juice samples, and the results demonstrated the potential of the synthesized DESs for the extraction and determination of contaminants in aqueous samples.
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BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 34
·期 3
·e4767
·
IF 1.748
Yong-hong Liu,Ting-ting Du,Jing-yuan Wan,Hua Zhao,Dan Huang,Jian-sha Li,Xin-hui Jiang
Disorders of certain branched-chain amino acids may be associated with the occurrence and development of non-alcoholic fatty liver disease. Measurement of related branched-chain amino acid levels could provide a reference for the clinical and scientific research of the non-alcoholic fatty liver disease. An established HPLC–FLD method was used to quantify aspartic acid, glutamate, glutamine, glycine, taurine, tyrosine, 4-amino butanoic acid, tryptophan, methionine, valine, phenylalanine, isoleucine and leucine in mouse brain tissue. Brain tissue samples mixed with internal standard (3-aminobutyric acid) were processed, then derivatized with 2- O -phthaldialdehyde, and finally separated on an ODS2 column through gradient elution at a flow rate of 1.0 ml·min −1 . The excitation and emission wavelengths were set at 340 and 455 nm, respectively. The mobile phase A was 100% methanol and the mobile phase B consisted of 30 mmol·L −1 sodium acetate (pH 6.8). The injection volume was 20 μl and the single run time was 45 min. Several parameters, accuracy, precision, and stability, were verified and the results showed the established method had good sensitivity and resolution for all of the 13 compounds and internal standard in mouse brain.
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JOURNAL OF CHEMICAL TECHNOLOGY AND BIOTECHNOLOGY
·
2019
·Vol. 94
·期 9
·2917-2927
·
IF 2.659
Zhuo Sun,Yang Lu,Lina Zhu,Wei Liu,Yue Qu,Nan Lin,Ping Yu
BACKGROUND Fluoroquinolone antibiotics and their metabolites can accumulate in soil and water. Trace amounts of fluoroquinolone antibiotic residues in the environment necessitate the pretreatment of samples prior to analysis. In this work, a polyoxyethylene cetyl ether (POELE20)–NaH 2 PO 4 aqueous two-phase system (ATPS) was combined with high-performance liquid chromatography (HPLC) to separate and determine trace quantities of ciprofloxacin (CIP), norfloxacin (NRF) and pefloxacin (PEF) in environmental samples. RESULTS Single-factor, multi-factor, reproducibility and accuracy experiments were performed. The extraction efficiencies and enrichment factors for the three antibiotics were above 90 and 13.8%, respectively, under optimal conditions. The recovery efficiency of CIP was 92.08–99.50%, with a relative standard deviation (RSD) of 0.60–6.34%, and the recovery efficiency of NRF and PEF was 93.40–99.30%, with RSD of 0.98–5.16%, when this method was applied to spiked water and soil samples. The RSDs of intra- and inter-day analyses were 1.56–3.42 and 1.33–3.97%, respectively. CONCLUSIONS This study demonstrated that POELE20–NaH 2 PO 4 ATPS coupled with HPLC was suitable for the simultaneous separation, concentration and determination of trace quantities of CIP, NRF and PEF in environmental samples. Moreover, this method can be applied for the determination of trace fluoroquinolone antibiotics in food samples. © 2019 Society of Chemical Industry
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MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 8
·1-8
·
IF 5.479
Qin Zucheng,Jiang Yanxiao,Piao Huilan,Tao Shuo,Sun Ying,Wang Xinghua,Ma Pinyi,Song Daqian
Halloysite nanotubes (HNTs) were functionalized with gold nanoparticles. The morphology and structures of this composite were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, powder X-ray diffraction, and surface area and pore-size analyses. The material was employed, in conjunction with a syringe pump and an organic filter head, to the enrichment of five triazines (atrazine, desmetryn, prometorn, tebumeton, ametryn) in spiked rice samples. Several parameters that may affect the extraction efficiencies, including type and volume of extraction solvent, amount of sorbent, times of ultrasonic extraction and adsorption, volume and flow rate of elution solvent, were optimized. Following elution with acetonitrile, the herbicides were quantified by using HPLC. Under the optimum conditions, the LODs of the method, when applied to spiked rice samples, are the range from 0.06 to 1.32 ng g −1 (LODs = 3SD/k). The relative intra-day and inter-day recoveries ranged from 80.6 to 106.5% and 80.4–107.3%, respectively, and relative standard deviations ranged from 0.8 to 8.7% and 3.6–9.6%, respectively.
Packed hybrids of gold nanoparticles and halloysite nanotubes (Au/HNTs) were prepared and applied to the dispersive solid-phase extraction by packed sorbent of five triazine herbicides from rice.
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Journal of Analytical Methods in Chemistry
·
2019
·
IF 1.589
Yong Zhang,Xian-Liang Zou,Yong-Li Wang,Lu Gao,Gui-Xin Chou
In this study, we used quantitative high-performance liquid chromatography equipped with an ultraviolet detector (HPLC-UV) and solid phase extraction (SPE) to determine the levels of four phenylethanoid glycosides and five triterpene acids in Liuwei Dihuang capsules (LDCs). LDCs were methanol-extracted and purified using a 500 mg/6 mL silica-based C18 SPE cartridge. Two elutions were analyzed on a ChromCore C18 column under two HPLC conditions. To improve the pretreatment clean-up, an array of silica- and polymer-based SPE cartridges were compared. Both wash and elution steps were also optimized to achieve the highest removal of impurities. Under optimal chromatographic conditions, good linearity was achieved for all compounds (correlation coefficient of r ≥ 0.999), with a quantification limit ranging from 0.0076 to 0.418 μg/mL. The method had satisfactory efficiency and reproducibility with recovery rates ranging from 91.6 to 99.3% with a relative standard deviation below 1.5%. Taken together, this demonstrated SPE as a suitable extension of HPLC-UV for the determination of phenylethanoid glycosides and triterpene acids in complex LDCs.
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MICROCHIMICA ACTA
·
2020
·Vol. 187
·期 1
·1-9
·
IF 6.232
Duo Huixiao,Li Yijing,Liang Xiaojing,Wang Shuai,Wang Licheng,Guo Yong
Magnetic hierarchical nickel/nickel oxide/carbon nanorods (Ni/NiO@C) were prepared via the pyrolysis of a metal-organic framework containing nickel(II) nickel (Ni-MOF; Ni 3 (BTC) 2 ) under argon atmosphere. In this material, magnetic Ni/NiO@C nanoparticles are embedded in porous carbon nanorods, and the morphology is similar to that of the original Ni-MOF precursor. The synthesized nanorods were applied as magnetic sorbents in the solid-phase extraction of five benzoylurea insecticides (flufenoxuron, chlorbenzuron, teflubenzuron, diflubenzuron and triflumuron), and their performance was evaluated under optimized conditions. The results show that the material exhibits high extraction recoveries from spiked samples (82.9%–107.6%) and linear response in the range of 0.2–450 μg·L −1 . It is also characterized by relatively low limits of detection (50–100 ng·mL −1 ) at a signal-to-noise ratio of 3. The sorbent is chemically stable and can be repeatedly recycled, with little decline in extraction capacity after 20 cycles of reuse. The method was successfully applied to the quantification of benzoylureas in tea, wolfberry, millet, and oat samples, and it showed high extraction efficiency.
Schematic representation of the synthesis of magnetic hierarchical nickel/nickel oxide/carbon nanorods derived from Ni-MOF. The material is employed as a sorbent for the magnetic solid-phase extraction of benzoylurea insecticides.
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PLoS One
·
2018
·Vol. 13
·期 6
·e0198515
·
IF 2.766
Jingyuan Shao,Wen Cao,Haibin Qu,Jianyang Pan,Xingchu Gong
The aim of this study was to present a novel analytical quality by design (AQbD) approach for developing an HPLC method to analyze herbal extracts. In this approach, critical method attributes (CMAs) and critical method parameters (CMPs) of the analytical method were determined using the same data collected from screening experiments. The HPLC-ELSD method for separation and quantification of sugars in Codonopsis Radix extract (CRE) samples and Astragali Radix extract (ARE) samples was developed as an example method with a novel AQbD approach. Potential CMAs and potential CMPs were found with Analytical Target Profile. After the screening experiments, the retention time of the D-glucose peak of CRE samples, the signal-to-noise ratio of the D-glucose peak of CRE samples, and retention time of the sucrose peak in ARE samples were considered CMAs. The initial and final composition of the mobile phase, flow rate, and column temperature were found to be CMPs using a standard partial regression coefficient method. The probability-based design space was calculated using a Monte-Carlo simulation method and verified by experiments. The optimized method was validated to be accurate and precise, and then it was applied in the analysis of CRE and ARE samples. The present AQbD approach is efficient and suitable for analysis objects with complex compositions.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2018
·
IF 2.831
Lan Luo,Congcong Gu,Mingxian Li,Xiangyuan Zheng,Feng Zheng
4-Nitrobenzaldehyde is the synthetic raw material and an important photodegradation product of chloramphenicol . With a structural “alert” of human genotoxic potential and reported mutagenicity, this compound should be controlled in drug substances as a potential genotoxic impurity. However, current analysis methods require complex pre-treatment processes and/or lack sufficient specificity and sensitivity. Nitrophenylhydrazine is a common carbonyl derivatization reagent used to determine the residual aromatic aldehydes in drug samples. In the present study, we report an unexpected advantage of 3-nitrophenylhydrazine hydrochloride as a derivatization reagent in the derivatization high-performance liquid chromatography-ultraviolet detection method to determine 4-nitrobenzaldehyde in chloramphenicol samples. Compared with other nitro-substituted phenylhydrazines , 3-nitrophenylhydrazine hydrochloride can minimize drug matrix and derivatization reagent interferences, since the maximum absorption wavelength of its derivative is significantly red-shifted to 397 nm. The derivatization conditions have been optimized in terms of reaction efficiency, including reaction temperature, time, and diluting solvent, through a design of experiments. As a result, after reaction with 500 μg mL −1 of 3-nitrophenylhydrazine hydrochloride in acetonitrile-water (70:30, v/v) at 60 °C for 30 min, the developed HPLC method could be used to determine 4-nitrobenzaldehyde with a limit of detection of 0.009 μg mL −1 . The method was then validated and applied for the determination of residual 4-nitrobenzaldehyde in chloramphenicol and its eye-drop samples.
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MICROCHEMICAL JOURNAL
·
2019
·
IF 3.206
Xin Fu,Dongliang Zhu,Lan Huang,Xiangyang Yan,Shaomin Liu,Chenghui Wang
A highly sensitive and selective method for the simultaneous extraction and determination of trace vanillin , ethyl vanillin , maltol and ethyl maltol in beverage samples using magnetic solid-phase extraction coupled with high-performance liquid chromatography (HPLC) was developed. The novel superparamagnetic dummy template molecularly imprinted polymers (Fe 3 O 4 @MDMIP) were prepared by adopting a sol-gel approach using 3-hydroxy-2,6-bis(hydroxymethyl) -4-pyrone, whose structure was similar to that of the vanillin and maltol, as the dummy template for selective extraction of vanillin, ethyl vanillin, maltol and ethyl maltol. The obtained Fe 3 O 4 @MDMIP exhibits high uniformity and monodispersity. Besides, Fe 3 O 4 @MDMIP has an outstanding magnetic susceptibility (56.33 emu g −1 ) than common obtained samples. The maximal adsorption capacity (Q max ) of the resulting Fe 3 O 4 @MDMIP for the four food additives was up to 609.99 mg g −1 . The imprinting factors of the Fe 3 O 4 @MDMIP ranged from 2.07 to 2.71 for the four food additives, which indicated that the obtained adsorbents have high selectivity. Under the optimum experimental conditions, the Fe 3 O 4 @MDMIP was successfully applied to the magnetic solid-phase extraction of vanillin, ethyl vanillin, maltol and ethyl maltol followed by HPLC determination in beverage samples. Validation experiments indicated that the developed method presented good linearity (2.07–463 ng mL −1 ), satisfactory precision (RSD, 2.68–6.91%), and high recovery (91.2–107.1%). The limits of detection ranged from 44 to 201 ng L −1 , and the enrichment factors were in the range of 432–484. The results demonstrated great potential of the optimized method for sample preparation in routine analysis of trace food additives.
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