FOOD CHEMISTRY
·
2022
·
IF 9.231
Can Zhang,Shuo Li,Jing Wu,Tengteng Ping,Ling Ma,Ke Wang,Kaoqi Lian
More and more attention has been paid to undesirable chemical contaminants from food raw materials and ingredients. The study aimed to fabricate novel hydroxyl-functionalized magnetic porous organic polymer Fe 3 O 4 @SiO 2 -NH 2 @Ph-POP and explore its use as magnetic adsorbents for magnetic solid-phase extraction (MSPE) for extracting 31 amide herbicides from fruit wine samples prior to high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Several operational parameters were optimized and the as-prepared magnetic polymer displayed favorable extraction efficiency. The method also showed low limits of detection (0.015–1.412 μg·L -1 ) and limits of quantitation (0.049–4.707 μg·L -1 ). Recoveries for all of the herbicides in four different spiked level samples were between 65.06 % and 101.95 % with intra-day and inter-day relative standard deviations less than 9.89 % and 10.54 %, respectively. The proposed MSPE-HPLC-MS/MS method was successfully applied to simultaneously determine 31 amide herbicides in fruit wine.
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MICROCHIMICA ACTA
·
2022
·Vol. 189
·期 9
·1-11
·
IF 6.408
Yang Yu-Ping,Chen Ji-Kai,Guo Ping,Lu Yan-Rui,Liu Cai-Fang,Wang Bang-Jin,Zhang Jun-Hui,Xie Sheng-Ming,Yuan Li-Ming
A spherical chiral porous organic polymer (POPs) COP-1 is synthesized by the Friedel–Crafts alkylation reaction of Boc-3-(4-biphenyl)-L-alanine (BBLA) and 4,4′-bis(chloromethyl)-1,1′-biphenyl (BCMBP), which was used as a novel chiral stationary phase (CSPs) for mixed-mode high-performance liquid chromatography (HPLC) enantioseparation. The racemic compounds were resolved in normal-phase liquid chromatography (NPLC) using n-hexane/isopropanol as mobile phase and reversed-phase liquid chromatography (RPLC) using methanol/water as mobile phase. The COP-1-packed column exhibited excellent separation performance toward various racemic compounds including alcohols, amines, ketones, esters, epoxy compounds, organic acids, and amino acids in NPLC and RPLC modes. The effects of analyte mass and column temperature on the separation efficiency of racemic compounds were investigated. In addition, the chiral resolution ability of the COP-1-packed column not only can be complementary in RPLC/NPLC modes but also exhibit a good chiral recognition complementarity with Chiralpak AD-H column and chiral porous organic cage (POC) NC1-R column. The relative standard deviations (RSD) ( n = 5) of the retention time, resolution value, and peak area by repeated separation of 1-(4-chiorophenyl)ethanol are all below 3.0%. The COP-1 column shows high column efficiency (e.g., 17,320 plates m −1 for 1-(4-chlorophenyl)ethanol on COP-1 column in NPLC), high enantioselectivity, and good reproducibility toward various racemates. This work demonstrates that chiral POPs microspheres are promising chiral materials for HPLC enantioseparation. Graphical abstract
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JOURNAL OF FOOD QUALITY
·
2022
·
IF 3.2
Yingqi Chen,Chonggao Hu,Jiaojiao Xu,Xiaodong Pan,Baifen Huang
In this paper, we built a method of verifying the 4 retinols of vitamin A and 8 tocopherol isomers of vitamin E in the food industry based on RP-HPLC-PDA-FLR. The effect of laboratory light conditions on the target components was considered for the first time, and it was found that the loss rate of the target components was the smallest in the case of a white laboratory bench with red or LED light in the dark room. There was no finding of extraction recoveries of the target components with a significant difference under different saponification conditions. Meanwhile, it was found that using ethyl acetate/n-hexane mixed solvent as the extraction solvent could ensure the effective extraction of the target components. Finally, baseline separation of 12 components was achieved within 45 min using the C30 column. With the help of methodological verification, we found that the recovery rate ranged from 76.45% to 93.52%, and RSD was between 0.19% and 12.99%; the Limit of Detection minimum value was 0.01 mg/100 g and the Limit of Quantitation minimum value was 0.03 mg/100 g. The detection method was successfully applied to the distribution detection of 4 kinds of retinols and 8 kinds of vitamin E in egg and dairy products and provided technical support for the accurate nutritional evaluation of vitamin A and vitamin E.
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RSC Advances
·
2021
·Vol. 11
·期 57
·35754-35764
·
IF 3.361
Ning Zhang,Siyu Guo,Bolin Gong
A bridged bis(β-cyclodextrin) ligand was firstly synthesized via a thiol–ene click chemistry reaction between allyl-ureido-β-cyclodextrin and 4-4′-thiobisthiophenol, which was then bonded onto a 5 μm spherical silica gel to obtain a novel bridged bis(β-cyclodextrin) chiral stationary phase (HTCDP). The structures of HTCDP and the bridged bis(β-cyclodextrin) ligand were characterized by the 1H nuclear magnetic resonance (1H NMR), solid state 13C nuclear magnetic resonance (13C NMR) spectra spectrum, scanning electron microscope, elemental analysis, mass spectrometry, infrared spectrometry and thermogravimetric analysis. The performance of HTCDP in enantioseparation was systematically examined by separating 21 chiral compounds, including 8 flavanones, 8 triazole pesticides and 5 other common chiral drugs (benzoin, praziquantel, 1-1′-bi-2-naphthol, Tröger's base and bicalutamide) in the reversed-phase chromatographic mode. By optimizing the chromatographic conditions such as formic acid content, mobile phase composition, pH values and column temperature, 19 analytes were completely separated with high resolution (1.50–4.48), in which the enantiomeric resolution of silymarin, 4-hydroxyflavanone, 2-hydroxyflavanone and flavanone were up to 4.34, 4.48, 3.89 and 3.06 within 35 min, respectively. Compared to the native β-CD chiral stationary phase (CDCSP), HTCDP had superior enantiomer separation and chiral recognition abilities. For example, HTCDP completely separated 5 other common chiral drugs, 2 flavanones and 3 triazole pesticides that CDCSP failed to separate. Unlike CDCSP, which has a small cavity (0.65 nm), the two cavities in HTCDP joined by the aryl connector could synergistically accommodate relatively bulky chiral analytes. Thus, HTCDP may have a broader prospect in enantiomeric separation, analysis and detection.
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MICROCHEMICAL JOURNAL
·
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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JOURNAL OF ENVIRONMENTAL SCIENCE AND HEALTH PART B-PESTICIDES FOOD CONTAMINANTS AND AGRICULTURAL WASTES
·
2021
·
IF 1.99
Zhongbei Zhang,Kai Ding,Zhou Lu,Nan Fang,Bo Wang,Zhiguang Hou,Zhongbin Lu
In the present study, an analytical method that combined a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method and high-performance liquid chromatography coupled with tandem mass spectrometry was developed to determine trifluorocide in fresh and dried ginseng roots, plants (stems and leaves), and soil. At three spiked levels (0.01, 0.1, and 1.0 mg kg−1), the mean recoveries (n = 15) of trifluorocide from fresh and dried ginseng roots, plants, and soil were in the range of 95.6 − 109.7%, with relative standard deviations less than 10.0%. The limits of quantitation of different matrices were determined to be 0.01 mg kg−1. Dissipation and residue study of trifluorocide was conducted in ginseng cultivation ecosystems in Northeast China. The t1/2 (half-life) of trifluorocide in ginseng fresh roots, plants, and soil were 8.3–13.1 days, 7.4–10.9 days, and 8.8–10.6 days, respectively. The terminal residues of trifluorocide in ginseng fresh roots were less than 0.01 mg kg−1 after 35 days of trifluorocide application. This study could be beneficial in residue analysis and assist in the scientific application of trifluorocide during ginseng cultivation.
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ACS Omega
·
2021
·
IF 3.512
Zhihui Lin,Yingnan Lin,Jianqi Lin,Yizhi Zhang,Song Fang
A modified QuEChERS method in combination with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was first developed for the determination of fenbutatin oxide in six types of samples (soil, tobacco, rice, milk, pork liver, and pork). Fenbutatin oxide was extracted with acetonitrile containing 1% formic acid (v/v) and purified by dispersive solid-phase extraction using primary secondary amine (PSA) and quantitatively analyzed by HPLC-MS/MS. In the range of 0.005–1 mg/kg, a good linear relationship exists between the concentration of fenbutatin oxide and the peak area, giving a coefficient of determination (R2) of >0.99. The recoveries of fenbutatin oxide at three spiked levels were 79.04–97.12% with the relative standard deviations (RSDs) of 3.30–10.96%, and the limit of quantification (LOQ) was 0.007 mg/kg. In addition, the developed method is consistent with the reference method (R2 = 0.9896, n = 40). The method is demonstrated to be convenient and reliable for the routine monitoring of fenbutatin oxide in soil and plant- and animal-derived foods.
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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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Food Analytical Methods
·
2021
·Vol. 14
·期 7
·1345-1358
·
IF 3.366
Wei Yihua,Zhang Jinyan,Qiu Shuyan,Huang Qingqing,Yuan Linfeng,Chen Liumeng,Dai Tingcan,Tu Tianhua,Zhang Biaojin,Yan Han,Li Weihong
A simple, rapid, and accurate method for determination of selenocystine (SeCys 2 ), methyl selenocysteine (MeSeCys), selenourea (SeUr), selenite (Se(IV)), selenotmethionine (SeMet), and selenate (Se(VI)) in grain crops was developed, based on the coupling of ion-pair reversed-phase high-performance liquid chromatography (IP-RP-HPLC) and ultraviolet irradiation hydride generation atomic fluorescence spectrometry (UV-HG-AFS). The conditions of IP-RP-HPLC-UV-HG -AFS were studied. The conditions of the pretreatment sample, such as types and dosage of proteinases, were investigated. The detection limits (LODs) for six Se species were between 0.77 and 1.77 μg·L −1 . Then, the proposed method has been successfully used to analyze selenium (Se) species in Se-enriched rice paddy ( Oryza sativa L. ), soybean ( Glycine max (Linn.) Merr. ), and sweet potato ( Ipomoea batatas (L.) Lam. ) with foliar application of sodium selenite solution. SeMet was the major Se spices in Se-enriched grain crops, ranged from 77–90% of the total Se contents. The capabilities of Se enrichment were relatively larger differences in three-grain corps as follows: soybean > rice paddy > sweet potato.
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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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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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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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