MICROCHEMICAL JOURNAL
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2021
·
IF 4.821
Piaoyang Li,Danmei Rao,Yimei Wang,Xiaorong Hu
Porous polythiophene materials were successfully synthesized by external-crosslinker method and applied as sorbents in solid-phase extraction. A method for the determination of tetracycline antibiotics (tetracycline/ oxytetracycline/doxycycline) in fish and chicken manure was proposed by combining solid phase extraction-ultraviolet visible spectrophotometer (SPE-UV) and solid phase extraction-high performance liquid chromatography (SPE-HPLC). The effects of material dosage, extraction time, washing time, eluent type and dosage, and the reusability of polythiophene sorbent on extraction rate were investigated. With the use of SPE-HPLC method, satisfied linearity for three tetracyclines antibiotics was obtained in the range of 0.004–1 mg/L. The detection limits (LODs) were ranged from 0.0012 to 0.0027 mg/L and the relative standard deviations (RSDs) were 3.5–7.3% (n = 5). The recoveries in actual fish samples and chicken manure samples were 91.1–114.1% and 69.5–93.2%, respectively. No tetracycline antibiotics were detected in fish samples and no doxycycline was detected in chicken manure samples. However, oxytetracycline and tetracycline were detected in two chicken manure samples with the contents of 5.12, 6.58 mg/kg and 6.08, 7.72 mg/kg, respectively. This method was simple, sensitive and suitable for the determination of tetracyclines in practical samples.
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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
·
2020
·
IF 2.34
Xin Huang,Zhiyi Du,Beiqi Wu,Liyan Jia,Xiaowen Wang,Xu Jing
In this paper, a dispersive liquid–liquid microextraction method based on the solidification of floating organic droplets, combined with high-performance liquid chromatography (DLLME-SFOD-HPLC), was developed for the detection of strobilurin fungicides (azoxystrobin, pyraclostrobin, and trifloxystrobin) in cereals. Natural fatty acids were used as an extractant and have low toxicity, density, and freezing point. The extractant nonanoic acid was evenly dispersed as droplets in sample solution and was then solidified in the upper layer of sample solution after centrifugation and ice bath, which improved the extraction and collection efficiency. The dispersive liquid-liquid microextraction procedure was optimised by univariate analysis and the Box-Behnken response surface methodology. Optimum conditions were as follows: the volume of nonanoic acid was 82 μL, the volume of acetonitrile was 620 μL, and the amount of salt was 256 mg. Under optimised conditions, the method had good linearity with a correlation coefficient higher than 0.997, and the limit of detection was 2.57–4.87 μg kg−1. The recoveries of azoxystrobin, pyraclostrobin, and trifloxystrobin in rice, corn, and wheat were 82.0%-93.2%, and the relative standard deviations were 1.6%-7.4%. Therefore, the method was successfully applied to detect target fungicides in cereals.
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JOURNAL OF AOAC INTERNATIONAL
·
2020
·Vol. 104
·期 2
·479-484
·
IF 1.51
Lan Tao,Yu Congcong,Li Ren,Ma Zheng,Xi Xingjun,Chu Qiao
BackgroundSolanesol is an important pharmaceutical intermediate raw material, mainly used to synthesize coenzyme Q10, vitamin K2. It can be found prominent in potato stems and leaves. But now potato stems and leaves are always abandoned or discarded as they are not suitable for use as feed in aquaculture or other purposes. These agricultural waste resources can be reutilized as the corresponding extracts.ObjectiveTo develop a simple and standardized method for the detection of total solanesol in potato leaves and its extracts.MethodsN-hexane was chosen as the extraction solvent for three times in the solanesol extraction from potato leaves. HPLC-MS was used for the detection.ResultsThe LOQ was 0.3 µg/g and the linear range was from 0.1 to 50 µg/mL. The precision and stability were evaluated by the relative standard deviations (RSDs) of three samples (potato leaves, Extract-1, Extract-2) for interday and intraday. The accuracy of the method was evaluated by the recoveries of three different spiked concentrations of solanesol for three samples, and results showed it ranged from 80.7% to 99.0% with RSDs less than 8.7%.ConclusionsThe method we established can provide a simple and standardized way for the extraction and detection of total solanesol.HighlightsThe work laid a foundation for the resource reutilization of potato stem and leaf.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2020
·Vol. 413
·期 1
·215-223
·
IF 3.637
Li Na,Zhao Tengwen,Du Li,Zhang Ziyang,Nian Qixun,Wang Manman
A graphitic carbon nitride (g-C 3 N 4 /Fe 3 O 4 )–based magnetic solid-phase extraction (MSPE) approach was established for fast and simple analysis of estrogens in milk powders. The composites were characterized by X-ray diffractometer, scanning electron microscope, and Brunauer-Emmett-Teller surface area and pore size distribution analyzer. Compared with the bulk g-C 3 N 4 , g-C 3 N 4 /Fe 3 O 4 gave a narrower distribution of mesopores and provided an enhanced surface area from 77.1 to 113.7 m 2 /g. Polar analytes of estrogens were selected as model compounds and the extraction of four estrogens was achieved in n-hexane using 15 mg of adsorbent within only 2 min. Possible extraction mechanism of g-C 3 N 4 /Fe 3 O 4 for these estrogens was explored in terms of the polarity of the analytes and the adsorption performance of the adsorbent. The hydrophobicity and the hydrogen-bond interaction between the estrogens and g-C 3 N 4 were responsible for the efficient adsorption. Combined with HPLC, MSPE with the prepared adsorbent gave the enhancement factors of 20 to 24 and the linear ranges of 2–200 μg/kg for 17 β -estradiol and 17 α -ethinylestradiol, 1.5–150 μg/kg for estrone, and 3–300 μg/kg for hexestrol. The detection limits and quantification limits for the estrogens in milk powders were 0.5–0.9 μg/kg and 1.5–3.0 μg/kg, respectively. The recoveries varied from 75.1 to 97.2%, with the intra-day and inter-day precisions ≤ 14.2%. Furthermore, the enrichment of the analytes and the clean-up of fat and protein interferences were achieved simultaneously with one-step g-C 3 N 4 -based MSPE. The present method was convenient, fast, and sensitive, and therefore could be successfully applied for the determination of estrogens in milk powders.
Graphical abstract
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Journal of Analytical Methods in Chemistry
·
2020
·
IF 1.878
Fang Tian,Qun-Jia Ruan,Ying Zhang,Hui Cao,Zhi-Guo Ma,Gai-Lian Zhou,Meng-Hua Wu
We aimed to establish a quantitative analysis method of six constituents (5-caffeoylquinic acid, 3-caffeoylquinic acid, 4-caffeoylquinic acid, 1,3-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid, and 4,5-dicaffeoylquinic acid) in Artemisia capillaris (Yinchen) and its decoction by using HPLC coupled with DAD. Besides, the transformation paths of the six constituents were analyzed in decoction preparation processing. The analytical method was fully validated in terms of linearity, sensitivity, precision, repeatability, and recovery and applied to assess the transformation trend and quantitative analysis of the six constituents in Yinchen decoction. The contents of six constituents varied greatly in Yinchen herb and Yinchen decoction, and there were inextricable internal relationships between them. Presumably 3-caffeoylquinic acid was isomerized to generate 5-caffeoylquinic acid and 4-caffeoylquinic acid. Similarly, 1,3-dicaffeoylquinic acid and 3,4-dicaffeoylquinic acid were produced by isomerization of 4,5-dicaffeoylquinic acid. In conclusion, this study provides a chemical basis for quality control of Yinchen decoction, and the changes of selected markers in decoction could give us some novel perspectives to study the relationship between substances and drug efficacy.
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MICROCHIMICA ACTA
·
2020
·Vol. 187
·期 4
·1-8
·
IF 6.232
Li Lin,Han Dandan,Wang Mingwei,Han Yehong,Yan Hongyuan
A composite was synthesized from two-dimensional molybdenum disulfide (MoS 2 ) nanosheets and hypercrosslinked polymers (HCP), and the composite was characterized by infrared spectroscopy, scanning electron microscopy, and specific surface area. The fluffy and porous structure and multiple adsorption sites (π-interaction, static electricity, hydrogen bonding) make it ideal for use as an adsorbent. A pipette tip solid-phase extraction with the composite as the adsorbent combined with HPLC–FLD was developed to determine trace amounts of polycyclic aromatic hydrocarbons (phenanthrene, anthracene, fluoranthene, pyrene, benzo(α)anthracene) in environmental water. Under optimal extraction conditions, the method has a wide linear range (0.5–100 ng mL −1 ) and low limit of detection (0.024–0.099 ng mL −1 ), and the recoveries of PAHs from spiked environmental water were 73.8% to 123.6% (relative standard deviation ≤ 6.7%, n = 3).
Schematic representation of a three-dimensional molybdenum disulfide–ethylenediamine–hypercrosslinked polymer composite (MoS 2 –EDA–HCP) using pipette tip solid-phase extraction adsorbent for extracting trace levels of polycyclic aromatic hydrocarbons (PAHs) prior to HPLC–FLD. HCP, hypercrosslinked polymer; MoS 2 , molybdenum disulfide; EDA, ethylenediamine
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BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 34
·期 2
·e4763
·
IF 1.748
Qing-ling Qi,Ya-Ming Yu,Cheng Tang
Target biomolecule-immobilized magnetic beads could be used as a powerful tool for screening active compounds present in natural products. Low damage rates of the target proteins, associated with the availability of diverse automated online approaches for analysis, make it a valuable tool for affinity studies. RAW264.7 cells (a kind of murine macrophage cell line) were used in this study. These cellular membranes were immobilized onto the surface of MBs and were used for screening the active compounds of Polygonatum sibiricum. Combining this technique with HPLC led to the identification of an active compound and its biological activity was confirmed. This is the first report establishing the use of RAW264.7 cellular membrane-coated magnetic bead fishing followed by HPLC analysis for screening active compounds from natural products.
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JOURNAL OF SEPARATION SCIENCE
·
2018
·Vol. 41
·期 22
·4115-4121
·
IF 2.415
Jie Li,Wangsheng Zeng,Xiaojing Lai,Xu Wang,Xin Xu,Hongping Cai,Lijun Wei,Xiang lei Cheng
A novel approach for the simultaneous and selective analysis of chlortetracycline, doxycycline, 4-epichlortetracycline, oxytetracycline, metacycline, and tetracycline by high-performance liquid chromatography coupled with sensitive post-column chemiluminescence reaction was set up. Six tetracyclines were separated through a simple and effective isocratic procedure using a mixture of acetonitrile and 3.5 mM methanesulfonic acid. After that, intensive chemiluminescence signals were produced by the reaction between cerium(IV) and methoxylated cypridina luciferin analogues system in the presence of tetracyclines. Under the appropriate experimental conditions, the developed method was evaluated by testing of linearity, limits of detection, precision, and accuracy. The limit of detection was from 2 to 10 nM and relative standard deviation of intraday precision was below 9%. The developed high-performance liquid chromatography with chemiluminescence method has been performed for the with trace analysis of tetracycline antibiotic residues in milk samples with satisfactory results.
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BIOMEDICAL CHROMATOGRAPHY
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2018
·Vol. 32
·期 11
·e4338
·
IF 1.688
Dan Huang,Qing-Song Jiang,Jun-Qing Yang,Ting Cui,Nian-Ru Wang,Ting-Ting Du,Xin-Hui Jiang
The determination of amino acids and monoamine with actions like neurotransmitters or modulators has become increasingly important for studying the relationship between the dysfunction of neurotransmitters and the pathogenesis of diabetic encephalopathy. Here, a high-performance liquid chromatography with fluorescence detection method was developed to simultaneously determine nine monoamines and amino acids including three excitatory neurotransmitters (aspartate, glutamate, and serotonin), four inhibitory neurotransmitters (glycine, γ -aminobutyric acid, taurine, dopamine), a precursor of 5-HT (tryptophan) and methionine using homoserine as the internal standard. The separation was performed on a BDS column with methanol-buffer solution of 35 mmol/L sodium acetate and 5 mmol/L citric acid (pH 6.0) using a simple gradient elution. Several parameters including specificity, precision, and recovery were validated after optimization of the analytical conditions. The developed method was successfully applied to determine the cortex and the hippocampus samples from Sprague–Dawley rats. Our results showed that various neurotransmitters involved in diabetes mellitus may tend to be differentially modulated and present a different alteration tendency at different time course, which might be associated with the duration of diabetes mellitus.
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TALANTA
·
2018
·
IF 4.244
Xuemei Wang,Pengfei Huang,Xiaomin Ma,Xinzhen Du,Xiaoquan Lu
A novel Estrone (E1) molecularly imprinted polymers (MIPs-E1)-coated solid-phase microextraction (SPME) fiber was prepared by in-situ polymerization on inner and outer surface of the capillary, namely MIPs-E1-coated in-out-tube SPME (MIPs-E1-IOT-SPME), which combines the advantages of enhanced extraction efficiencies of IOT-SPME and specific adsorption abilities of MIPs, and shows nearly double enrichment capacity compared to in-tube SPME (IT-SPME). The extraction conditions were optimized and a method for determination six endocrine disrupting compounds (EDCs) by MIPs-E1-IOT-SPME coupled with HPLC is developed. The MIPs-E1 coating was characterized by fourier-transform infrared spectrometry (FTIR), scanning electron microscopy (SEM), N 2 adsorption-desorption and Thermal gravimetric analysis (TGA). Under the optimum condition, the MIPs-IOT-SPME-HPLC method shows low limits of detection (LODs) (0.21–0.80 μg L −1 ) and limits of quantification detection (LOQs) (0.69–2.6 μg L −1 ), wide linear ranges from 10.0 to 1000 μg L −1 for each compound with exception of E2 and E3 from 20.0 to 1000 μg L −1 , and acceptable reproducibility of one fiber for five parallel determinations is 2.4–6.6% (RSD) and fiber-to-fiber is 4.5–8.1% (RSD). The satisfactory recoveries are in the range of 88.5–105.1% with good RSDs less than 7.9% at the five spiked levels of 20.0, 50.0, 80.0, 200.0 and 500.0 μg L −1 . Moreover, when compared with commercial fibers, the MIPs-E1-IOT-SPME fiber displays excellent adsorption capacity and specific selectivity .
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Food Analytical Methods
·
2018
·Vol. 12
·期 2
·381-393
·
IF 2.245
Sun Xiao-Dong,Wu Hai-Long,Liu Zhi,Chen Yue,Liu Qian,Ding Yu-Jie,Yu Ru-Qin
A rapid and sensitive analytical strategy combining high-performance liquid chromatography-diode array detection (HPLC-DAD) and chemometrics methods was developed for the determination of multi-class food additives in a variety of beverage samples. Different kinds of beverages, which contain diverse unknown interferences, can be directly injected into a chromatographic system after a simple dilution or pretreatment step, and the data were recorded in a short time under a simple gradient elution mode. Although peaks overlapped and changeable interferences existed in the dimension of the chromatographic and spectral in real beverages, all food additives were accurately resolved by using a second-order calibration method based on alternating trilinear decomposition (ATLD) algorithm, and accurate chromatographic profiles, spectral profiles, and concentration profiles were also obtained. Limits of detection for all additives were between 1.40 and 165.1 ng mL −1 , while limits of quantitation ranged from 4.20 to 500.2 ng mL −1 . The spiked recoveries were in the range of 87.3–103% (except amaranth) with RSDs less than 10.2%. Compared with the results obtained by classic HPLC method, our proposed method was more accurate. In all, the proposed method is fast, sensitive, and universal and could be used as a reliable tool to determine food additives and quality monitoring in different complex beverages.
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JOURNAL OF SEPARATION SCIENCE
·
2013
·Vol. 36
·期 8
·1343-1348
·
IF 2.591
Qiuyun Wang,Yajin Xiong,Baozhu Lu,Jun Fan,Sheng Zhang,Shengrun Zheng,Weiguang Zhang
N -(2,4-dinitrophenyl)-proline and N -(2,4-dinitrophenyl)-serine were enantiomerically resolved on the BSA chiral stationary phase by HPLC in reversed-phase mode. Effects of chromatographic conditions on enantioseparation and elution order have been investigated in detail. For these two samples, reversal of enantiomer elution order was observed by changing buffer pH, the content of acetonitrile, or alcohol modifiers in mobile phase, which is firstly reported in the BSA chiral stationary phase studies. More interestingly, combined effect between buffer pH and the content of acetonitrile was also observed. In addition, coelution range of enantiomers varied along with the content of acetonitrile in mobile phase.
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危险品化学品经营许可证（带存储）