MICROCHEMICAL JOURNAL
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2026
·
IF 5.2
Wanning Li,Xiangjie Kong,Mengting Fu,Yike Han,Shuo Xie,Penghui Li,Liyun Kong
An in situ DES-LLME/HPLC-DAD method was developed for detecting trace quinolones in wastewater. • Quinolones were used as hydrogen bond acceptors for in situ DES formation. • The method showed good linearity with low LODs of 0.094–0.905 μg/L and satisfactory recoveries. • The method was applied to real samples, confirming its potential for antibiotic monitoring. Background Quinolone antibiotics are widely used in human and veterinary medicine due to their broad-spectrum antibacterial activity and cost-effectiveness. However, their environmental persistence and frequent occurrence in aquatic systems have raised concerns regarding potential ecological risks. Accurate risk assessment requires sensitive analytical methods capable of detecting trace levels of quinolones in complex environmental matrices. Traditional preconcentration techniques like solid-phase extraction and liquid-liquid extraction face several limitations including high-cost sorbents, sorbent degradation, memory effects, labor-intensive procedures, large solvent consumption, and the use of toxic organic solvents. Results To address these challenges, we developed a sensitive method for the determination of trace quinolones in water samples by integrating in-situ deep eutectic solvent-based liquid-liquid microextraction with high performance liquid chromatography coupled with a diode array detector. A key innovation of this approach lies in the utilization of the target quinolones as hydrogen bond acceptors during in situ DES formation, enabling direct extraction from aqueous media. Through theoretical screening using the conductor-like screening model for real solvents (COSMO-RS) and subsequent experimental verification, butyl 4-hydroxybenzoate was identified as the optimal hydrogen bond donor. Under the optimized extraction conditions, enrichment factors ranged from 33.43 to 66.50, with corresponding extraction recoveries of 33.43–66.50%. The method demonstrated satisfactory sensitivity, with limits of detection ranging from 0.094 to 0.905 μg/L, good linearity with determination coefficients exceeding 0.99, high accuracy with recoveries of 82.25%–122.08%, and acceptable precision with relative standard deviations below 13.76%. Application to real wastewater samples successfully detected enrofloxacin (20–39 μg/L) and moxifloxacin (20 μg/L), confirming the practical feasibility of the proposed method. Significance This in situ deep eutectic solvent-based liquid-liquid microextraction method offers a rapid, sensitive and efficient approach for monitoring quinolone antibiotics in aquatic environments. Its innovative design not only enables effective determination of quinolones but also holds considerable promise for developing novel in-situ DES enrichment strategies aimed at detecting other emerging environmental pollutants in complex matrices, thereby offering substantial potential for environmental monitoring and risk assessment. Download: Download high-res image (133KB) Download: Download full-size image
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高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2013
·Vol. 36
·期 19
·3277-3284
·
IF 2.591
Gao Xia,Fan Jing,Zhu Guifen,Wang Xiaolong,Wang Jianji
A novel 1-butyl-3-methylimidazolium chloride ionic liquid surface imprinted solid-phase sorbent was synthesized. The as-prepared material was characterized by SEM, Brunauer–Emmett–Teller surface area analysis and Fourier Transform IR measurements. Then its adsorption properties for alkyl imidazolium ionic liquids, including adsorption capacities, adsorption kinetics, and properties of selective separation and enrichment were studied in detail. It was shown that the ionic liquid surface imprinted polymer exhibited high selective recognition characteristics for the imidazolium chloride ionic liquids with short alkyl chains (C n mimCl, n = 2, 4, 6, 8) and the adsorption equilibrium was achieved within 25 min. Various parameters were optimized for the 1-butyl-3-methylimidazolium chloride ionic liquid surface imprinted polymer SPE column, such as flow rate, eluent solvent, selectivity, and reusability of the column. Then, the SPE column coupled with HPLC was used for the determination of alkyl imidazolium ionic liquids. Experimental results showed that the existence of their structural analogs and common concomitants in environmental matrices did not affect the enrichment of 1-butyl-3-methyl imidazolium chloride ionic liquid. The average recoveries of 1-butyl-3-methylimidazolium chloride ionic liquid in spiked water samples were in the range of 92.0–102.0% with the RSD lower than 5.8%.
研究领域:
分析化学
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环境科学
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高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
Yaming Sun,Baoen Su,Ke Zhang,Yuhong Lin,Bing Wang,Min Sun
The monitoring of phthalates (PAEs) is essential for ensuring the quality and safety of Chinese Baijiu. However, the complex matrices and low level pose significant technical challenges. Herein, an online in-tube solid-phase microextraction coupled with high-performance liquid chromatography-diode array detector (IT-SPME-HPLC-DAD) was proposed for detecting PAEs in Baijiu. A covalent organic framework was grown onto carbon fibers, then the material was carbonized to get another fibers (CFs@C-COF). The CFs@C-COF as a sorbent of IT-SPME demonstrated enhanced physicochemical properties, including highly a graphitized structure with mild defects, a high surface area, abundant mesopores and excellent durability. The superior extraction efficiency of CFs@C-COF for PAEs can be ascribed to multiple interactions, such as hydrophobic, π-stacking, and pore-filling effects. The developed online IT-SPME-HPLC-DAD method exhibited the linear ranges (1.0–10.0, 1.5–10.0 μg L −1 ), the limits of detection (0.3–0.5 μg L −1 ), acceptable relative recoveries (72.7 %–125.8 %), and satisfactory repeatability. In addition, the total duration of this online extraction procedure was only 23 min and no any pretreatment of the samples was required except for diluting Baijiu samples. This research not only offered a simple and effective strategy for the analysis of Baijiu but also expanded the application of carbonized COFs in food safety.
研究领域:
食品安全
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分析化学
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PubMed
高影响因子
PLANT CELL TISSUE AND ORGAN CULTURE
·
2024
·Vol. 156
·期 2
·1-11
·
IF 2.3
Zhang Gaowei,Luo Liping,Tian Kaili,Ning Fangjian,Wu Dong,Sun Qifang,Yu Wenjie,Yi Shengxiang,Hao Yingbin
Dendrobium officinale is a perennial herb with medicinal and edible qualities. The growth and nutritional properties of this plant are significantly affected by the light quality. However, the impact of varying light quality on the phytochemical characteristics of tissue-cultured seedlings of D. officinale is still unknown. In this study, tissue-cultured seedlings of D. officinale were grown for ninety days under six LED lights, including white light (W), blue LED (B), red LED (R), and three composite light environments with varying quantities of red and blue light: 1:2 (R1B2), 1:1 (R1B1), and 2:1 (R2B1). The growth status and physiological signs of the seedlings were analyzed and we used high-performance liquid chromatography (HPLC), ultra-performance liquid chromatography/time-of-flight mass spectrometry (UPLC-Q/TOF-MS), and pathway enrichment analysis to thoroughly examine the metabolomic changes, with a focus on phenolic compounds. Our results indicated that R2B1 illumination led to the best growth of D. officinale seedlings, with maximal energy absorption, and phenolic contents. In conclusion, R2B1 was considered the most profitable for tissue-culture production of D. officinale .
研究领域:
植物学
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药用植物学
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代谢组学
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高影响因子
Asian Journal of Pharmaceutical Sciences
·
2016
·Vol. 12
·期 2
·202-208
·
IF 0
Huiyan Shi,Chenzhi Hou,Liqiang Gu,Zhe Wei,Hang Xing,Meiyu Zhang,Shixiao Wang,Longshan Zhao,Kaishun Bi,Xiaohui Chen
The present study was designed to investigate the influence of the pretreatment of piperazine ferulate on pharmacokinetic parameters of methotrexate in methotrexate-induced renal injury rats. A simple and efficient high performance liquid chromatography coupled with mass spectrometry (HPLC-MS) method was developed to determine methotrexate in rat plasma. Methotrexate and syringic acid (internal standard) were extracted from rat plasma samples by protein precipitation with acetonitrile. The analysis was performed on a CAPCELL PAK C 18 column (150 mm × 4.6 mm, 5 µm) with acetonitrile and 5 mmol/l ammonium acetate aqueous (10:90, v/v ). The linear range was 5.0 × 10 −2 to 100.0 µg/ml for methotrexate. Other parameters were all within the acceptance criteria. The validated method was successfully applied the pharmacokinetic study of methotrexate between two methotrexate treated groups (with and without the pretreatment of piperazine ferulate). Compared with the methotrexate treated alone group, the pharmacokinetic parameters in the methotrexate with the pretreatment of piperazine ferulate group showed significantly lower MRT (0-t) , MRT (0-∞) and T 1/2 . Results suggested that methotrexate can be rapidly eliminated, cleared or metabolized in rat blood, which might be related to the pretreatment of piperazine ferulate. The method provided deeper insights into rational clinical use of methotrexate with the pretreatment of piperazine ferulate on cancer patients with renal dysfunction.
研究领域:
药理学
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药物代谢
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肾脏病学
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肿瘤学
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临床药学
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分析化学
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BIOMEDICAL CHROMATOGRAPHY
·
2014
·Vol. 29
·期 6
·869-875
·
IF 1.662
Yonggang Chen,Junhua Meng,Jili Zou,Jing An
Hordenine is an active compound found in several foods, herbs and beer. In this work, a novel sorbent was fabricated for selective solid-phase extraction (SPE) of hordenine in biological samples. The organic polymer sorbent was synthesized in one step in the plastic barrel of a syringe by a pre-polymerization solution consisting of methacrylic acid (MAA), 4-vinylphenylboronic acid (VB) and ethylene glycol dimethacrylate (EGDMA). The conditions for preparation were optimized to generate a poly(MAA-VB-EGMDA) monolith with good permeability. The monolith exhibited good enrichment efficiency towards hordenine. By using tyramine as the internal standard, a poly(MAA-VB-EGMDA)-based SPE-HPLC method was established for analysis of hordenine. Conditions for SPE, including volume of eluting solvent, pH of sample solution, sampling rate and sample volume, were optimized. The proposed SPE-HPLC method presented good linearity ( R 2 = 0.9992) within 10–2000 ng/mL and the detection limits was 3 ng/mL, which is significantly more sensitive than reported methods. The method was also applied in plasma and urine samples; good capability of removing matrices was observed, while hordenine in low content was well extracted and enriched. The recoveries were from 90.6 to 94.7% and from 89.3 to 91.5% for the spiked plasma and urine samples, respectively, with the relative standard deviations <4.7%. Copyright © 2014 John Wiley & Sons, Ltd.
研究领域:
分析化学
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生物分析
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分离科学
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药物分析
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高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 15
·3074-3085
·
IF 2.557
Lingfei Han,Desheng Hou,Congyu Ma,Na Fu,Jing Liu,Feng Feng,Wenyuan Liu,Feng Zheng
Short-chain aliphatic amines are a class of hazardous impurities in drug substances. A simple method, involving derivatization followed by high-performance liquid chromatography with diode array detection, has been developed for residue determination of eight aliphatic amines simultaneously in drug substances. Different halonitrobenzenes derivatization reagents were systematically compared. As a result, 1-fluoro-2-nitro-4-(trifluoromethyl)benzene was selected since the derivatization effectively shifted the absorption wavelength to the visible region (400–450 nm), where most drug substances, impurities and even the derivatization reagent absorb very weakly. Due to the redshift effect, interference was minimized and adequately low limits of quantitation were reached (0.24–0.80 nmol/mL). Moreover, the derivatization reaction was readily carried out in dimethyl sulfoxide at room temperature for 1 h using N , N -diisopropylethylamine as catalyst to achieve the highest yield. Without any pre-treatment, the derivatives were analyzed by high-performance liquid chromatography with diode array detection. The high stability of the derivatives within 24 h at room temperature (RSD<1.04%) further facilitated the simultaneous preparation and consecutive analysis of quantities of samples. Finally, the proposed method was successfully applied for residue determination of eight aliphatic amines simultaneously in eight drug substance samples. This study could be helpful for the routine analysis and residue control of aliphatic amines in drug substances.
研究领域:
药物分析
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分析化学
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杂质谱分析
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色谱学
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Xueyun Wei,Lanrui Yang,Zhuomin Zhang,Gongke Li
Trace disinfection by-products (DBPs) in aquatic products may have serious impact on human health via direct or indirect consumption. However, the accurate and sensitive quantification of trace chlorophenol DBPs in complex aquatic products still remains a great challenge. In this work, the defective MIL-101(Fe)-NH 2 enrichment medium was prepared for developing a selective membrane solid phase extraction (M-SPE) technology for quantifying trace chlorophenol DBPs in fish, coupled with high performance liquid chromatography-ultraviolet-visible spectroscopy (HPLC-UV). The established analytical method showed good selectivity, sensitivity and accuracy, achieving the limits of detection from 0.03 to 0.15 ng/mL and the recovery from 80.0% to 117%, achieving sensitivity comparable to that of HPLC-mass spectrometry (MS)-based methods. The validated method was successfully applied to quantify chlorophenol DBPs in grass carp and crucian carp, offering a selective and sensitive alternative for monitoring chlorophenol DBPs in fish, with practical advantages for routine analysis via compatibility with widely available HPLC-UV.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2026
·Vol. 40
·期 7
·e70526
·
IF 1.7
Shu-Zhen Chen,Yong-Lin Ma,Dong-Xiao Li,Lian-Lin Yang,Ji-Wen Wang,Qian-Qian Hu,Hong-Liang Ma
This study developed an online HPLC-ABTS method to screen antioxidant phenolic acids in Pandani tectorii radix et rhizoma (PT) from 20 geographical origins. Six common constituents were screened and assigned by standards: neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, isochlorogenic acid B, isochlorogenic acid A, and isochlorogenic acid C. Using these six components as variables, four regression models were constructed to predict ABTS radical scavenging rate: support vector regression (SVR), decision tree regression, K-nearest neighbors (KNN) regression, and extreme gradient boosting (XGBoost) regression. From 80 samples, 64 were used for model development, and 16 were reserved for hold-out validation. Model selection employed 5-fold, nested, and leave-one-out cross-validations, complemented by permutation tests and learning curve analysis. The SVR model performed best, with nested CV R 2 = 0.9298, RMSE = 4.1207, MAE = 2.2313, and an optimism gap of 0.0137. After final tuning (C = 100, gamma = 0.1, and epsilon = 0.5), it achieved R 2 = 0.9000, RMSE = 4.0602, and MAE = 2.2986 on the hold-out set. This efficient and accurate method enables simultaneous screening of antioxidant constituents and prediction of radical scavenging activity, providing a new technical tool and scientific basis for PT quality evaluation.
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高影响因子
Journal of Analytical Methods in Chemistry
·
2022
·
IF 2.594
Yuhuang Wu,Liyan Li,Guxu Ming,Xinyue Ma,Changfu Liang,Yonghui Li,Xiaoning He
A rapid, sensitive, selective, and accurate HPLC–MS/MS method was developed and validated for the simultaneous determination of chlorogenic acid, naucleactonin C, khaephuoside A 3,4-dimethoxyphenyl-1-O-β-apiofuroseyl(1 ⟶ 2)-β-D-glucopyranoside in rat plasma and tissues after oral administration of Nauclea officinalis extracts. Chloramphenicol was used as an internal standard (IS). The plasma and tissue samples were extracted by protein precipitation with methanol-ethyl acetate (1 : 1, v/v) including 0.1% (v/v) formic acid. The chromatographic separation was achieved by using an C18 column with gradient elution using mobile phase, which consisted of 0.1% formic acid water (A) and acetonitrile (B) and the flow rate of 0.8 mL/min. Mass spectrometric detection was performed in multiple reaction monitoring (MRM) mode utilizing electrospray ionization (ESI) in negative mode. The developed method exhibited good linearity (determination coefficients, R2 ≥ 0.9849), and the lower limits of quantification were 2, 5, 5, and 25 ng/mL for chlorogenic acid, naucleactonin C, khaephuoside A, and 3,4-dimethoxyphenyl-1-O-β-apiofuroseyl(1 ⟶ 2)-β-D-glucopyranoside. The intraday and interday precisions (relative standard deviation, RSD) were less than 12.65%, while the accuracy was ranged from 86.31 to 114.17%. The recovery rate were 51.85–97.06%, 75.99–106.68%, 77.46–105.35%, and 68.36–103.75% for chlorogenic acid, naucleactonin C, khaephuoside A, and 3,4-dimethoxyphenyl-1-O-β-apiofuroseyl(1 ⟶ 2)-β-D-glucopyranoside the matrix effects were 50.17–116.62%, 86.75–115.99%, 45.79–87.44%, and 51.60–92.34% for chlorogenic acid, naucleactonin C, khaephuoside A, and 3,4-dimethoxyphenyl-1-O-β-apiofuroseyl(1 ⟶ 2)-β-D-glucopyranoside in different matrix. The developed method was successfully applied to a pharmacokinetic study and tissue distribution of four compounds in rats after oral administration of Nauclea officinalis extracts.
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PubMed
高影响因子
TALANTA
·
2023
·
IF 6.1
Qingying Wang,Lianfang Chen,Xiaoyan Cui,Jie Zhang,Yaohui Wang,Xiupei Yang
Herein, a covalent organic framework (COF) was grown on a magnetic metal-organic framework (MOF) by a solvothermal method for the efficient extraction of bisphenols (BPs). The magnetic solid-phase extraction (MSPE) of four bisphenols (bisphenol A, bisphenol B , bisphenol AF and bisphenol C) was carried out without adjusting the pH and salt concentration. When 30 mg Fe 3 O 4 @NH 2 -MIL-88(Fe)@TpPa was used to adsorb for 25 min, 6 mL methanol was used to elute for 20 min, and the extract was detected by high-performance liquid chromatography (HPLC). The proposed method has a low detection limit of 0.011–0.036 ng mL −1 , a wide linear range of 0.05–100 ng mL −1 , and a correlation coefficient (R 2 ) of 0.9980–0.9998. The intra-day and inter-day precisions are 0.74–2.54% and 1.68–3.72%, respectively. Bisphenol A was determined by applying the proposed method to the determination of actual milk samples. The standard addition experiment showed that the relative recovery of the four bisphenols was 85.70–119.7%. Pseudosecond-order, first-order, Langmuir and Freundlich models were applied to explore the adsorption characteristics of Fe 3 O 4 @NH 2 -MIL-88(Fe)@TpPa. In general, the established Fe 3 O 4 @NH 2 -MIL-88(Fe)@TpPa-MSPE-HPLC-UV method exhibits attractive sensitivity, simple manipulation, and excellent reusability, and it has excellent prospects for the detection of trace BPs in complex milk matrices.
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高影响因子
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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高影响因子
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