JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 18
·3710-3717
·
IF 2.557
Xinyu Liang,Juntao Wang,Juanjuan Wu,Qiuhua Wu,Chun Wang,Zhi Wang
A three-dimensional graphene was synthesized through a hydrothermal reaction of graphene oxide with phytic acid. The microstructure and morphology of the phytic acid induced three-dimensional graphene were investigated by nitrogen adsorption–desorption isotherms, scanning electron microscopy, and transmission electron microscopy. With a large surface area and three-dimensional structure, the graphene was used as the solid-phase extraction adsorbent for the extraction of phthalate esters from bottled water and sports beverage samples before high-performance liquid chromatographic analysis. The results indicated that the graphene was efficient for the solid-phase extraction of phthalate esters. The limits of detection (S/N = 3) of the method for the analytes were 0.02–0.03 ng/mL for the water samples and 0.03–0.15 ng/mL for the sports beverage sample. The limits of quantitation (S/N = 9) for the analytes were 0.06–0.09 ng/mL for water samples and 0.09–0.45 ng/mL for sports beverage sample. The calibration curves for the phthalate esters by the method had a good linearity from 0.1 to 80.0 ng/mL with correlation coefficients larger than 0.9997. The recoveries of the analytes for the method fell in the range of 86.7–116.2% with the relative standard deviations between 1.5 and 6.8%.
研究领域:
分析化学
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环境科学
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产品关联
DOI
PubMed
高影响因子
RSC Advances
·
2025
·Vol. 15
·期 21
·16973-16982
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IF 4.6
Haijun Wang,Qiao Zhang,Xiaolin Li,Huan Chen,Xiaolan Zhu,Liming Yang,Hongling Yin,Jing Sun,Shuhong Fang,Hui Zhang
A large-volume direct-injection (LVDI) method was developed and validated for the simultaneous analysis of 69 antibiotics in bottled water using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Target antibiotics included 23 sulfonamides, 19 quinolones, 12 macrolides, 11 β-lactams, and 4 tetracyclines. Optimization of ion source parameters led to enhanced signal intensities for 55 antibiotics. The 100 μL injection volume was both feasible and preferred, resulting in increased signal intensities while maintaining unchanged peak shapes for the antibiotics. Good absolute recoveries for the 69 antibiotics were obtained with the LVDI method, primarily ranging from 80% to 120%, whereas lower absolute recoveries of macrolides, quinolones, sulfonamides and β-lactams were observed with a solid-phase extraction (SPE) method. The limits of detection (LODs) for antibiotics were generally comparable between the LVDI and SPE methods, with values below 1 ng L−1 for most antibiotics (0.00271–26.6 ng L−1). Analysis of 25 brands of bottled water using the LVDI method revealed the presence of 54 antibiotics from 5 classes, with detection frequencies (DFs) ranging from 4% to 100% and detected concentrations between 0.0453 and 37.4 ng L−1. Multiple antibiotics were detected simultaneously in bottled water, with more than 10 antibiotics identified in each of 9 different brands. Quinolones and sulfonamides were the predominant antibiotics, accounting for over 80% of the total concentration. Only sulfaclozine showed significantly different concentrations between purified drinking water and natural mineral water (22.2 vs. 17.2 ng L−1, p < 0.05).
研究领域:
分析化学
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环境科学
·
食品科学
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产品关联
DOI
PubMed
高影响因子
CHROMATOGRAPHIA
·
2024
·
IF 1.2
Huang Zhongping,Wu Ermiao,Shi Dongliang,Zhang Jingkun,Shen Zhenlu,Zheng Ruixing,Shen Jian
The quantification analysis of microplastics (MPs) in bottled water, purified tap water and branded table salt was executed by double-shot pyrolysis–gas chromatography/mass spectrometry (Py–GC/MS), and the concentration was expressed as a mass concentration, which was more suitable for the data comparison. MPs including polymethyl methacrylate (PMMA), polyethylene terephthalate (PET), polycarbonate (PC), polypropylene (PP), polystyrene (PS) and polyethylene (PE) were separated by filtration with glass fiber filter membranes. After being folded, the whole glass filter membrane containing MPs was transferred into a pyrolysis cup directly to avoid the sample loss during transfer. The characteristic pyrolysates were used to identify and quantify PMMA, PET, PC, PP, PS and PE. The linear relationships were found between the polymer weight amount and peak areas of each characteristic pyrolysates with the correlation coefficients larger than 0.993. The intra-day precisions of the pyrolysates for peak areas were 0.56–18.94%, and the inter-day variability was 8.47–19.88%. The recovery values of the spiked standards were in a range of 81.5–114.5%. MPs in bottled water, purified tap water and branded table salt samples were successfully quantified by the proposed Py–GC/MS method. For four brands of bottled water samples, 0.088 μg/L PET was found in one sample. PP was detected in all purified tap water samples from five brands with the concentrations between 0.028 and 0.489 μg/L, and PE was detected in purified tap water samples from two brands with the concentrations between 0.194 and 1.26 μg/L. As for nine table salt samples, PP were found in a range of 4.00–182.80 μg/100 g salt in eight table salt samples. Due to the high content of MPs in purified tap water samples and large daily consumption, the estimated daily intake (EDI) of MPs from purified tap water was calculated. The estimated daily intakes (EDIs) for adults are 2.57 ng PP/kg/d and 4.17 ng PE/kg/d from purified tap water; the EDIs for children are 5.63 ng PP/kg/d and 9.11 ng PE/kg/d from purified tap water.
研究领域:
环境科学
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分析化学
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DOI
高影响因子
Food Analytical Methods
·
2022
·Vol. 15
·期 4
·1107-1117
·
IF 3.498
Wei Liulin,Liu Jie,Liu Qian,Chen Xiaomei,Li Zhiqiang,Xu Yidong,Gao Xueyun,Lu Xiaoxiao,Guo Zhian,Zhao Jingchan
In this study, a convenient and sensitive method for the determination of phthalate esters (PAEs) in plastic bottled water was proposed by on-line in-tube solid-phase microextraction (IT-SPME) coupled with high-performance liquid chromatography (HPLC). A hybrid monolithic column was synthesized with octamethacrylate substituted polyhedral oligomeric silsesquioxane (POSS-MA) as cross-linker and N-butyl methacrylate (BMA) as functional monomer, which was utilized as the extraction phase of IT-SPME. A number of important extraction parameters were systematically optimized, such as sampling flow rate, desorption solvent flow rate and volume, sample volume, and sample pH value. Under the optimal experimental conditions, the linear ranges of five PAEs were in the range of 0.1–60 ng mL −1 . The limits of detection were between 0.052 and 0.10 ng mL −1 , and the limits of quantification were less than 0.33 ng mL −1 . In addition, the intra-day and inter-day relative standard deviations of the method were 0.98–3.0% and 2.0–4.3%, respectively. The EFs of the method for five PAEs were more than 538. The proposed method was also successfully applied to analyze trace PAEs in real samples with good recoveries. The recoveries of this method ranged from 84.6 to 111.6% and the relative standard deviations were less than 4.5%. The extraction recoveries of the prepared hybrid monolithic column of the target PAEs did not decrease significantly within 60 cycles. The results showed that the on-line IT-SPME-HPLC method was sensitive, highly efficient, and operationally convenient.
研究领域:
分析化学
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环境科学
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Yu Du,Weiyi Jin,Siyu Yang,Yeqing Jia,Xinghua Li,Jianping Li,Mingyue Zhang,Yi Zhang
Bisphenol analogues (BPs) are a class of typical environmental endocrine disruptors (EDCs) that have recently attracted increasing attention with regard to their potential effects on human health. The objective of this study was to develop a method using a magnetic soft material, which consisted of hydrophilic deep eutectic solvent (DES) and magnetic multi-walled carbon nanotubes (MMWCNTs), for the dispersive solid-phase extraction (d-SPE), coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), for the determination of the levels of nine BPs in bottled water. The hydrophilic DES enable the rapid dispersion of MMWCNTs when the material is injected rapidly into the sample solution using a pipette gun. This process can therefore be completed in a relatively short period of time, resulting in an efficient extraction. Under optimal conditions, the limit of detections (LODs) of the method were 0.0003–0.003 μg/L and the limit of quantifications (LOQs) were 0.001–0.01 μg/L. The relative standard deviations (RSDs) of the method were only 2.42–7.59 % for inter-day and 3.71–9.67 % for intra-day. The method demonstrated good reproducibilities and recoveries, rendering it suitable for the determination of BPs in large-volume water samples.
研究领域:
环境科学
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分析化学
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毒理学
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Qiao Feng Wang,Ming Sun,Jiang Bing Sun,Jun Zhou
A novel and efficient method of surfactant-assisted temperature-controlled solidification ionic liquid dispersion liquid–liquid microextraction (SA-TCS-IL-DLLME) has been developed for the preconcentration and determination of trace five phthalate esters in bottled water. The analysis was completed by ultra-high performance liquid chromatography (UHPLC). In this study, hydrophobic low-density solid quaternary phosphonate ionic liquid ([P 44412 ] BF 4 ) was used as extractant while surfactant Tergitol TMN-6 was employed as dispersant. The dispersion of the extractant in the sample solution was promoted by water bath and vortex. At the same time, the temperature was controlled to transform the extractant from liquid to solid. Then, the separation of the extractant and the sample solution was achieved. Incidentally, extraction of the analyte was also finished. Important parameters which affected SA-TCS-IL-DLLME efficiency, such as the type and volume of extractant and dispersant, the amount of salt, the vortex time and pH value were investigated and optimized by single factor experiments. Under these optimized conditions, the method exhibited linearity ranges of 0.01–1.0 ng mL −1 with correlation coefficients between 0.9994 and 0.9998. The method’s intra-day ( n = 6) and inter-day ( n = 6) precision levels were maintained at ≤ 3.37 %, which was considered to be within acceptable limits. The computed detection and quantification limits were 16.54–24.60 and 54.91–82.04 ng mL −1 , respectively. Above all, this optimized method was effectively employed to extract five phthalate esters from bottled water with recoveries ranging from 94.83 % to 98.72 %. It can be used for rapid analysis and detection of phthalate esters in bottled water samples.
研究领域:
分析化学
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环境科学
·
食品科学
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产品关联
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2022
·Vol. 45
·期 23
·4224-4235
·
IF 3.614
Ruozhu Xu,Yuan Tao,Wang Yao,Honglin Qin,Lizhen Qiao
In this study, three-dimensional flower-like tin disulfide materials were prepared, and a highly efficient dispersive solid-phase extraction method was developed using the obtained three-dimensional tin disulfide adsorbents for the preconcentration and determination of six endocrine-disrupting phenols in combination with high-performance liquid chromatography-ultraviolet detection. Several important experimental parameters influencing extraction efficiency were investigated, including the amount of adsorbent, ultrasound time, sample solution pH, sample volume, type of elution solvent, desorption time, and the number of desorption times. Under the optimized experimental conditions, the developed method showed good linearity with the determination coefficients of 0.993–0.998 in the linear range of 0.5–400 ng/ml and low limits of detection in the range of 0.15–1.0 ng/ml, as well as satisfactory intra-day and inter-day precisions with relative standard deviations of 0.1–9.8%. Finally, the proposed method was successfully applied for the enrichment and determination of trace endocrine-disrupting phenols in milk, tea beverage, and plastic bottled water samples, and acceptable recoveries were obtained from 70.1% to 119.1% under four different spiked concentration levels. The results showed that the three-dimensional tin disulfide materials had great potential for the extraction of endocrine-disrupting phenols contaminants in environmental and food samples.
研究领域:
分析化学
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环境科学
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食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
·
2016
·
IF 1.878
Fang Liu,Chang-Ying Hu,Quan Zhao,Yu-Jie Shi,Huai-Ning Zhong
Three nanocopper/low-density polyethylene (LDPE) composite films were tested in food simulants (3% acetic acid and 10% ethanol) and real food matrices (rice vinegar, bottled water and Chinese liquor) to explore the behaviours of copper migration using ICP-OES and GFAAS. The effects of exposure time, temperature, nanocopper concentration and contact media on the release of copper from nanocopper/LDPE composite films were studied. It was shown that the migration of copper into 10% ethanol was much less than that into 3% acetic acid at the same conditions. With the increase of nanocopper concentration, exposure time and temperature, the release of copper increased. Copper migration does not appear to be significant in the case of bottled water and Chinese liquor compared with rice vinegar with a maximum value of 0.54 μg mL−1 for the CF-0.25# bags at 70°C for 2 h. The presence and morphology of copper nanoparticles in the films and the topographical changes of the films were confirmed by field emission scanning electron microscope (FE-SEM) and atomic force microscope (AFM). In this manner, copper nanoparticles of different morphologies, sizes and distribution were found, and samples with higher nanocopper concentration had a more irregular topography. In the case of Fourier transform infrared spectroscopy (FTIR), no chemical bonds formed between copper nanoparticles and LDPE. Copper nanoparticles were just as physically dispersed in LDPE.
研究领域:
材料科学
·
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）