MOLECULES
·
2020
·Vol. 25
·期 6
·1415
·
IF 3.267
Rui Song,Qincheng Chen,Lili Yan,Pinhua Rao,Peng Sun,Lumei Wang,Guoqing Shen
Antibiotics and hormones widely exist in fertilizers and manures, which are excessively used in agriculture and animal husbandry. Considering their potential harm to the environment and human health, the detection of antibiotics and hormones has become a necessity. However, current methods find it difficult to simultaneously extract and detect antibiotics and hormones in soil and to maintain a high level of accuracy and a low cost. In this study, a straightforward, convenient, and simultaneous extraction and detection method of a representative antibiotic (sulfamethoxazole, SMZ) and hormone (17β-Estradiol, E2) in soil has been established. Ultrasound-assisted extraction (UAE) was used in the pretreatment process and high-performance liquid chromatography with the ultraviolet detector (HPLC-UV) method was then chosen in the detection process. By means of single factors and response surface experiments, optimal extraction conditions were a 41-mL buffer solution (pH 4.27) mixed with 1 g of soil sample, an ultrasonication time of 36 min, an ultrasonication temperature of 25 °C, and two extraction cycles. The detection limits of 0.3–10 μg/kg and quantification limits of 1–30 μg/kg have been obtained. Finally, the optimized simultaneous extraction and detection method was validated by three different real soil samples with recoveries ranging from 79.49% to 86.47%.Keywords:antibiotics;hormone;ultrasound-assisted extraction;HPLC-UV;response surface methodology
研究领域:
环境科学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
Talanta Open
·
2025
·
IF 3.7
Amna Naz,Sadia Haider,Mavra Rana,Neelum Malik,Attia Afzal,Muhammad Farooq,Muhammad Sarfraz
Oleanolic acid (OA) and apigenin (APG) demonstrate a wide range of pharmacological effects, including antioxidant, anti-inflammatory, antiviral, antidiabetic, hepatoprotective, and cardioprotective activities. Both compounds show anticancer potential and have been used individually to treat various cancer types, creating a rationale for their combined use. However, quantifying both drugs in quality and plasma samples presents challenges due to differences in their physicochemical properties and absorption wavelengths (OA: 210-215 nm, APG: 212, 269, and 337 nm). We developed and validated a novel High-Performance Liquid Chromatography UV detection (HPLC-UV) method to address this problem. Using a C18 column (4.6 mm x 250 mm, packing L1, 5 µm particle size) and a mobile phase of acetonitrile: methanol: tetrahydrofuran: water (60:20:8:12, v/v) with a detection wavelength of 215 nm. The method achieved retention times of 4.7 and 10 minutes for OA and APG in quality samples, and 4.9 and 9.8 minutes in plasma samples, respectively. The plasma sample was prepared by simple protein precipitation step. All validation parameters, including sensitivity, selectivity, precision, accuracy, robustness, and stability, met the required criteria. The validated HPLC-UV bioanalytical method was effectively applied in quantification, stability, and pharmacokinetic studies of co-loaded nanoformulations of OA and APG with particle size 163 nm and entrapment efficiency up to 93 %, establishing it as a promising analytical technique for detecting these anticancer agents in complex matrices such as blood, plasma, and polymeric systems.
研究领域:
药理学
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分析化学
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肿瘤学
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产品关联
DOI
高影响因子
SEPARATION AND PURIFICATION TECHNOLOGY
·
2015
·
IF 3.091
Xiao-Hui Yao,Dong-Yang Zhang,Ming-Hui Duan,Qi Cui,Wen-Jing Xu,Meng Luo,Chun-Ying Li,Yuan-Gang Zu,Yu-Jie Fu
A group of green solvent named polyols-based deep eutectic solvents (PDES) combined with microwave assisted extraction (MAE) was first successfully applied in extracting phenolic compounds from pyrola. A series of PDES with mixing different ratios choline chloride (ChCl) to different polyols were investigated for extraction, and ChCl/1,4-Butanediol (1/4) was found to be the suitable extraction solvent. MAE was more effective than heat-stirring extraction and ultrasonic assisted extraction with PDES. The extraction parameters were optimized by BBD test combined with response surface methodology. The optimal extraction conditions were 30% of water in ChCl/1,4-Butanediol (1/4) at 70 °C for 20 min and liquid/solid ratio 10 mL/g. Moreover, RP-HPLC-UV was developed for the determination of five main active components in pyrola. This method exhibited satisfactory linearity ( R 2 > 0.999), precision (RSD < 4.03%) and recovery (96.17–103.25%). Sample analysis showed that the contents of hyperin, 2′-O-galloylhyperin, quercitrin, quercetin-O-rhamnoside and chimaphilin in pyrola were 1.627, 4.958, 0.041, 0.089 and 0.349 mg/g, respectively. These results revealed that PDES would be promising green solvents for analytical sample preparation from plant herbs.
研究领域:
植物化学
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分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2024
·
IF 4
Jian-Jun Zhong,Lingling Zhao,Yuanxin Guo,Zhanming Li,Hua Ye,Huanan Guan,Zhiqiang Xing,Weiqing Wang
The coffee phytochemical trigonelline and its roasting products nicotinic acid and N -methylpyridinium represent an important class of bioactives that mediate the health benefits of coffee consumption. However, there is a paucity of methods for their simultaneous analysis in coffee beans, especially those affordable and reliable for widespread routine use. To improve this situation, an easy-to-use HPLC−UV method was developed in this study based on a reversed-phase/cation-exchange mixed-mode column showing unique chromatographic selectivity toward the polar and ionic analytes over the matrix components of coffee. The selectivity was achieved by using a decreasing acetonitrile gradient, which tuned the column to a cation-exchange/hydrophilic interaction (CEX/HILIC) mixed separation mode whilst minimizing its hydrophobic interaction capability. The method was assessed for figures of merit, giving limits of detection in coffee beans at around the 0.1 mg/100 g wet matter level, and verified for its applicability to a heterogeneous set of coffee bean samples differing in roasting degree and origin.
研究领域:
分析化学
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食品科学
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植物化学
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产品关联
DOI
高影响因子
Food Analytical Methods
·
2020
·Vol. 13
·期 8
·1673-1680
·
IF 2.667
Cheng Zhu,Ran Qin,Liu Jie,Deng Xing,Qiu Huidong,Jia Zhengfu,Su Xiaodong
Preservatives and sweeteners are always added in the food production process, which can extend the life and flavor of food. Benzoic acid and saccharin sodium are commonly used as preservatives and sweeteners respectively. Phenyllactic acid as a natural preservative, mainly produced by phenylalanine fermentation, may exist in fermented food. The objective of the current study is to develop a reverse-phase HPLC-UV method for simultaneous determination of benzoic acid, sorbic acid, phenyllactic, phenylalanine, and saccharin sodium in vinegar. They were separated on Sapphiresil TM (C 18 ) column (250 × 4.6 mm, 5 μm) with a mobile phase consisting of methyl alcohol:ammonium acetate buffer (pH 6.44; 0.02 M) (20:80, v/v) ran in isocratic mode at a flow rate of 1 mL/min. Complete baseline separation of five analytes was achieved in < 12 min, the linear range was 0.25–50 μg/mL with a correlation coefficient R 2 value > 0.9975, the method was validated with recoveries in the 96.93 to 118.42% range, and RSD was 0.39–6.21%. The detection limits of phenylalanine, benzoic acid, saccharin sodium, sorbic acid, and phenyllactic acid were 0.25, 0.01, 0.01, 0.025, and 0.05 mg/L. This method could be used for determining of benzoic acid, sorbic acid, phenyllactic acid, phenylalanine, and saccharin sodium in vinegar.
Graphical abstract
研究领域:
食品科学
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分析化学
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食品安全
✓ 已验证
DOI
高影响因子
CHEMOSPHERE
·
2018
·
IF 4.427
Junjie Ao,Jiaping Gu,Tao Yuan,Dan Li,Yuning Ma,Zhemin Shen
A highly selective sample cleanup method using molecularly imprinted polymers (MIP) was developed for the enrichment of domoic acid (DA, an amnesic shellfish toxin) from both seawater and shellfish samples. Molecular modelling was firstly applied to screening a suitable functional monomer and optimize the polymer preparation. Theoretical results were in a good agreement with those of the experimental studies. MIP was prepared by precipitation polymerization using 1, 3, 5-pentanetricarboxylic acid and 2-(Trifluoromethyl)acrylic acid as the template molecule and functional monomer, respectively. The morphology and molecular structure of MIP were revealed by scanning electron microscope (SEM) and fourier transform infrared spectroscopy (FTIR), respectively. The obtained MIP showed high affinity and selectivity for DA with binding site numbers of 0.875 mg g −1 and an average association constant of 0.219 L mg −1 evaluated by adsorption experiments. The developed molecularly imprinted solid-phase extraction (MISPE) column achieved satisfied adsorption rate (99.2%) and recovery (71.2%) with relative standard deviation (RSD) less than 1.0%, which is more stable and precise than the C 18 , SAX, and HLB columns. Finally, the determination method for DA in both seawater and shellfish samples was then successfully established and validated using MISPE coupled with high-performance liquid chromatography-ultraviolet detection (HPLC-UV). The method limit of detection was 20 μg L −1 and 50 μg kg −1 for seawater and shellfish, respectively. This study demonstrates that molecular modelling is a useful tool to screening functional monomer and optimize polymer preparation. It provides an innovative polymer for trace DA monitoring in both seawater and shellfish.
研究领域:
分析化学
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环境科学
·
海洋生物学
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Xin Di,Zhi Zhang,Yan Yang,Xiaoli Guo
A simple and sensitive homogeneous liquid–liquid microextraction based on switchable hydrophilicity solvent (SHS-HLLME) has been developed for fast enrichment and determination of pyrethroid insecticides in wolfberry samples via HPLC-UV. In HLLME, N, N-dimethylbenzylamine (DMBA) was used as SHS that can reversibly convert between water-insoluble and water-soluble states by applying CO 2 as trigger. Two phase separation was easily achieved by addition of NaOH solution without need of time-consuming of salting-out or forming ionpair, greatly shortening extraction time (3 min). The influencing extraction parameters were investigated and optimized in detail. Under the optimal condition, the method shows good linearity (1.0–200 ng/mL), low limits of detection (0.2–0.5 ng/mL), desirable precision (RSD < 9.8%) and accuracy (RE < 8.7%) and acceptable extraction recovery (71.4%-94.1%). The work provides a novel alternative approach for determination of pyrethroid insecticides at the low nanogram per microliter range with desirable sensitivity.
研究领域:
分析化学
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食品科学
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环境科学
✓ 已验证
产品关联
DOI
高影响因子
Analytical Methods
·
2014
·Vol. 6
·期 5
·1563-1568
·
IF 1.938
Huang Yang,Li Kang,Shao Hui Kai,Liu Sheng Quan,Xiang Fei Jun
A method using molecularly imprinted solid-phase extraction combined with RP-HPLC-UV was developed for determination of liquiritin (LQR) in rat plasma after oral administration of Compound Liquorice Tablets (CLTs). To this end, molecularly imprinted polymers were prepared by in situ polymerization, using LQR as the template, acrylamide as the functional monomer, and ethylene glycol dimethacrylate as the crosslinker, whose solid-phase extraction properties for liquiritin were evaluated by HPLC-UV. The enrichment and extraction recovery were investigated in the study after the extraction procedure was optimized. The recovery was larger than 85.0% and the RSD was less than 10.0%. The calibration curve was expressed as y = 16 004x − 1.864 (r = 0.996) with a linear range of 0.007–1.683 μg mL−1. Besides, the Tmax was 0.5 h for liquiritin and the Cmax was 0.8 μg mL−1 after oral administration of compound liquorice tablets. In addition, the pharmacokinetic parameters were calculated using a two-compartment model. The results indicated that the monolithic polymer pipette presented a good extraction efficiency for liquiritin. At the same time, the results indicated that the index components could basically reveal the pharmacokinetic behavior. This study was aimed to explore an approach that could be applied to promulgate the pharmacokinetics and provide more information for clinical applications.
研究领域:
药理学
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分析化学
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生物医学工程
✓ 已验证
产品关联
DOI
高影响因子
BIOTECHNOLOGY AND APPLIED BIOCHEMISTRY
·
2023
·Vol. 70
·期 6
·1806-1816
·
IF 2.8
Jing Zhou,Si-Jia Miao,Shi-Zhong Yang,Jin-Feng Liu,Hong-Ze Gang,Bo-Zhong Mu
Rhamnolipid, as a low-toxic, biodegradable and environmentally friendly biosurfactant, has broad application prospects in many industries. However, the quantitative determination of rhamnolipid is still a challenging task. Here, a new sensitive method for the quantitative analysis of rhamnolipid based on a simple derivatization reaction was developed. In this study, 3-[3′-( l -rhamnopyranosyloxy) decanoyloxy] decanoic acid (Rha-C10-C10) and 3-[3′-(2′- O -α- l -rhamnopyranosyloxy) decanoyloxy] decanoic acid (Rha-Rha-C10-C10) were utilized as the representative rhamnolipids. Liquid chromatography–mass spectrometry and high-performance liquid chromatography-ultra violet results showed that these two compounds were successfully labeled with 1 N1-(4-nitrophenyl)-1,2-ethylenediamine. There was an excellent linear relationship between rhamnolipid concentration and peak area of labeled rhamnolipid. The detection limits of the Rha-C10-C10 and Rha-Rha-C10-C10 were 0.018 mg/L (36 nmol/L) and 0.014 mg/L (22 nmol/L), respectively. The established amidation method was suitable for the accurate analysis of rhamnolipids in the biotechnological process. The method had good reproducibility with the relative standard deviation of 0.96% and 0.79%, respectively, and sufficient accuracy with a recovery of 96%–100%. This method was applied to quantitative analysis of 10 rhamnolipid homologs metabolized by Pseudomonas aeruginosa LJ-8. The single labeling method was used for the quantitative analysis of multiple components, which provided an effective method for the quality evaluation of other glycolipids with carboxyl groups.
研究领域:
生物技术
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分析化学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
BIOTECHNOLOGY LETTERS
·
2017
·Vol. 39
·期 8
·1229-1235
·
IF 1.73
Wang Qianqian,Xu Yixiang,Xu Jiaqi,Wang Xudong,Shen Chen,Zhang Yan,Liu Xiufeng,Yu Boyang,Zhang Jian
Objectives To characterize glycosyltransferases from Bacillus subtilis ATCC 6633 and investigate their substrate specificity towards plant polyphenols. Results Among the cloned and expressed six UDP-glycosyltransferases (BsGT1-6), BsGT-1 showed activity with a wide range of polyphenols: morin, quercetin, alizarin, rehin, curcumin and aloe emodin. The gene of BsGT-1 has an ORF of 1206 bp encoding 402 amino acids. The recombinant enzyme was purified to homogeneity by Ni–NTA affinity chromatograph, and its biochemical characteristics were identified by HPLC–UV/MS, 1 H-NMR and 13 C-NMR. BsGT-1 has an MW of approx. 46 kDa as indicated by SDS-PAGE; its activity was optimal at 40 °C and pH 8.5. The Km value of BsGT-1 towards morin was 110 μM. Conclusions BsGT-1 from B. subtilis was cloned. It had high catalytic capabilities towards polyphenols which would make it feasible for the structural modification of polyphenols.
研究领域:
生物化学
·
分子生物学
·
酶学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Qianqian Cai,Tianyu Zhao,Lianjun Zhang,Pan Zhao,Yajie Zhu,Haiyan Xu,Xiaohong Hou
Dispersive micro-solid-phase extraction (DMSPE) combined with dispersive liquid–liquid microextraction based on the solidification of a floating organic droplet (DLLME-SFO) was successfully developed for extraction and depuration of pantoprazole in rat plasma. The remarkable metal organic framework (MOF), MIL-101(Cr) was used as DMSPE adsorbent. The detection of pantoprazole was performed by convenient HPLC-UV. In the extraction of pantoprazole from plasma samples, small molecule compounds, including the target and abundant impurities, were easily admitted into the porous structure of MIL-101 (Cr) material in DMSPE; while, macromolecular compounds were handily excluded from the adsorbent. Next, the depuration process was achieved by removal of small polar impurities in DLLME-SFO. Influential factors were systematically optimized for ideal enrichment and depuration efficiency. Under the optimal conditions, a satisfactory linearity range from the lower limit of quantification (LLOQ, 100 ng/L) to 10 000 ng/L with the correlation coefficients ( r ) of 0.9934 was obtained. The LLOQ was 100 ng/mL and the relative recoveries were ≧ 73.2 ± 4.8%. The approving reproducibility, acceptable accuracy, and stability were all within the acceptance limits. This proposed method presented the advantages of environment-friendly, low-cost, recyclable, low impurity, and preferable applicability. It could offer a new idea for the pretreatment and pharmacokinetic study of pantoprazole in rat plasma.
研究领域:
分析化学
·
药物代谢动力学
·
医学检验
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE
·
2023
·Vol. 104
·期 1
·257-265
·
IF 4.1
Jie Zhao,Zi-Yu Li,Chun-Xu Yang,Ya-Ping Li,Yu-Shen Liu,Zhen Hua Hu,Xiao-Ming Pan,Xiu-Li Ma,Wei Wang,Xiao-Shuai Yang,Lu-Liang Wang
BACKGROUND Phenolic endocrine-disrupting chemicals (EDCs) are widespread and easily ingested through the food chain. They pose a serious threat to human health. Magnetic solid-phase extraction (MSPE) is an effective sample pre-treatment technology to determine traces of phenolic EDCs. RESULTS Magnetic covalent organic framework (COF) (Fe 3 O 4 @COF) nanospheres were prepared and characterized. The efficient and selective extraction of phenolic EDCs relies on a large specific surface and the inherent porosity of COFs and hydrogen bonding, π–π, and hydrophobic interactions between COF shells and phenolic EDCs. Under optimal conditions, the proposed magnetic solid-phase extraction-high-performance liquid chromatography–ultra violet (MSPE-HPLC-UV) based on the metallic covalent organic framework method for phenolic EDCs shows good linearities (0.002–6 μg mL −1 ), with R 2 of 0.995 or higher, and low limits of detection (6–1.200 ng mL −1 ). CONCLUSION Magnetic covalent organic frameworks (Fe 3 O 4 @COFs) with good MSPE performance for phenolic EDCs were synthesized by the solvothermal method. The magnetic covalent organic framework-based MSPE-HPLC-UV method was applied successfully to determine phenolic EDCs in beverage and water samples with satisfactory recoveries (90.200%–123%) and relative standard deviations (2.100%–12.100%). © 2023 Society of Chemical Industry.
研究领域:
环境科学
·
分析化学
·
材料科学
✓ 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）