ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2025
·
IF 3.8
Xu Jiaqi,Li Qianyu,Li Wenrui,Wu Di,Wu Yongning,Li Guoliang
Matrix effects pose a significant challenge in food analysis for the quantitative analysis of complex food samples. Herein, a novel magnetic covalent organic framework nanocomposite and the copper(I)-catalyzed azide–alkyne cycloaddition (CuAAC) click reaction-based stable isotope labeling (SIL) method were presented for highly selective and sensitive detection of steroid hormones in food samples using HPLC-MS/MS. The nanocomposite, Fe 3 O 4 @TAPB-COF, with a core–shell structure exhibited high adsorption capacities for steroid hormones. Combined with a SIL method based on the CuAAC click reaction, steroid hormones were accurately quantified in food samples with high sensitivity and selectivity. A pair of SIL agents, N -(2-azidoethyl)aniline (d 0 -NAEA) and d 5 - N -(2-azidoethyl)aniline (d 5 -NAEA), was synthesized to label steroid hormones in the samples and standard solutions, respectively. The labeling reaction is highly specific, and the formation of the derivatives is easily ionized by MS, thus overcoming matrix effects. More surprisingly, the ionization efficiency of steroid hormones increased by a factor of 4 to 56, with matrix effects ranging from 87.3 to 99.3%. Under optimal conditions, this method exhibited a low limit of detection (LOD) ranging from 0.1 to 2.6 μg L −1 and overcame the interference of matrix effects for trace-level steroid hormone analysis in foodstuffs.
研究领域:
分析化学
·
食品安全
·
生物医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
PeerJ
·
2019
·
IF 2.353
Hongli Yin,Ji Ma,Jichun Han,Maoru Li,Jing Shang
Background Quercetin (Qr), isoquercitrin (IQ), and quercetin-3-O-β-D-glucuronide (QG) are powerful phytochemicals that have been shown to exhibit disease prevention and health promotion properties. However, there may exist transformations between Qr, IQ, and QG in vivo . And the pharmacokinetic profiles of Qr, IQ, and QG have not been systematically compared. The pharmacokinetics study would be helpful to better understand the pharmacological actions of them. Methods Herein, we developed a reliable HPLC-MS method to compare the pharmacokinetics of Qr, IQ, and QG after separate (50 mg/kg) oral administration of them in rats, using puerarin as internal standard. The detection was performed using negative selected ion monitoring. This method was validated in terms of selectivity, linearity, precision, accuracy, extraction recovery, matrix effect, and stability; and shows reliabilities in monitoring the pharmacokinetic behaviors of these three compounds. Results Our results showed that after separate oral administration of Qr, IQ, and QG, all of the compounds could be detected in plasma. In addition, QG could be detected in the Qr group; Qr and QG could be measured in the IQ group; and Qr could be found in rat plasma after 1.5 h of QG administration. Moreover, the AUC 0− t of Qr in the; Qr group (2,590.5 ± 987.9 mg/L*min), IQ group (2,212.7 ± 914.1 mg/L*min), and QG group (3,505.7 ± 1,565.0 mg/L*min) was larger than the AUC 0− t of QG in the; Qr group (1,550.0 ± 454.2 mg/L*min), IQ group (669.3 ± 188.3 mg/L*min), and QG group (962.7 ± 602.3 mg/L*min). The AUC 0− t of IQ was the lowest among all groups. Discussion Quercetin, IQ, and QG can all be absorbed into plasma. A mutual transformation exists between Qr and QG, and IQ can be metabolized into Qr and QG in SD rats. These results would provide a meaningful basis for understanding the pharmacological actions of these three compounds.
研究领域:
药理学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2026
·
IF 3.4
Cui’e Qi,Jiaqi Song,Longwei Lv,Yidi Yin,Siyao Wang,Meng Li,Qing Li
A robust HPLC method employing a polysaccharide-based chiral stationary phase was developed and optimized for the enantiomeric separation of tetrahydrojatrorrhizine. Investigations into the effects of chromatographic conditions on enantiomeric separation revealed that a specific mobile phase, comprising methanol and ammonium acetate solution, significantly enhanced enantioselectivity with a resolution of 1.89 at a lower column temperature. Thermodynamic analysis based on van’t Hoff plots was carried out, which demonstrated a clear enthalpy-driven potential for chiral recognition, suggesting binding interactions played the dominant role in enantiomeric separation. To elucidate molecular mechanisms of chiral recognition, the complementary docking simulation was also performed, identifying that the observed enantioselectivity originated from differences in the key interactions, including hydrogen bond, π-π stacking, and steric hindrance. Additionally, a chiral HPLC-MS/MS method was fully validated for the determination of tetrahydrojatrorrhizine enantiomers in rat plasma, and applied to a preliminary enantioselective pharmacokinetic study. The results showed significantly different pharmacokinetic profiles between the two enantiomers, highlighting that the area under the curve of S -(−)-tetrahydrojatrorrhizine was statistically higher than that of R -(+)-tetrahydrojatrorrhizine. The integrated work presented herein provided a reliable analytical method and mechanistic insights into chiral recognition of tetrahydrojatrorrhizine enantiomers, supporting the precise evaluation of enantiomeric behaviors in vivo .
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2014
·
IF 2.694
Xin Liu,Yuan Hong,Qing He,Kai Huang
A simple, rapid and sensitive high-performance liquid chromatography–tandem mass spectrometric (HPLC–MS/MS) method was developed and validated for determining lycorine in rat plasma. Plasma samples were prepared by a simple protein precipitation with methanol containing dextrorphan as internal standard. The chromatographic separation was performed on a Kromasil 60-5CN column (3 μm, 2.1 mm × 150 mm) with the mobile phase of methanol/water (containing 0.1% formic acid) (40:60, v/v) at a flow rate of 0.2 mL/min, the total analytical runtime was 5 min. The detection was performed on a triple quadrupole tandem mass spectrometer equipped with Electronic Spray Ion by selected reaction monitoring (SRM) of the transitions at m / z 288.1 → 147.1 for lycorine and m / z 258.1 → 157.2 for dextrorphan, respectively. The calibration curve was linear over the range of 1–1000 ng/mL with the lower limit of quantification of 1 ng/mL for lycorine. The intra- and inter-day precision (R.S.D.%) were less than 8.5% and accuracy (R.E.%) was within ±7.0%. Lycorine was sufficiently stable under all relevant analytical conditions. This method was successfully applied to the pharmacokinetic study of lycorine in rats after intraperitoneal administration with different doses of 5, 10 and 20 mg/kg.
研究领域:
分析化学
·
药物代谢动力学
·
毒理学
✓ 已验证
DOI
高影响因子
JOURNAL OF FOOD BIOCHEMISTRY
·
2018
·Vol. 42
·期 3
·e12517
·
IF 1.552
Jiao-Jiao Yuan,Jun-Ling Tu,Frank G. F. Qin,Yong-Jun Xu,Bing Li
Oleuropein is an antioxidant olive constituent, but it is liable to degrade into hydroxytyrosol. Oleuropein extract was hydrolyzed by hemicellulase and the results presented that 14 phenols were identified in the ethyl acetate extract of enzymatic hydrolysate by HPLC-MS. Antioxidant activities (DPPH, ABTS, total reducing power, FRAP, and Fe 2+ chelating ability) of phenols were all added with the samples concentration increased, and dose–effect relationship also existed. 14 phenols all possessed certain inhibition effect against selected bacteria, and they had better inhibition effect against tested Gram-positive bacterium ( Staphylococcus aureus ) than Gram-negative bacterium ( Escherichia coli ). Finally, hydroxytyrosol, oleuropein, eugenol, caffeic acid, and 3,4-dihydroxybenzoic acid could present excellent antioxidant and antibacterial effect, and the two activities mainly had close relationship. Practical applications From the previous study we could know enzymatic biotransformation from oleuropein to HT was a promising method. Therefore, HT preparation from enzyme has attracted great attention of researcher. If that, a lot of enzymatic hydrolysate would be produced in the process. So, present study was to use fully the ethyl acetate extract of enzymatic hydrolysate, and to determine the chemical composition of phenolic compounds in EAE by HPLC-MS, and to evaluate their antioxidant and antimicrobial capacity. The result was shown that phenols of oleuropein extract after enzymatic process, therefore, may be suitable as a source of powerful antioxidants and bacteriostatic due to their stronger antioxidant and antibacterial activities. They could be widely applied in functional food industry for preservation.
研究领域:
食品科学
·
植物化学
·
生物技术
✓ 已验证
产品关联
DOI
高影响因子
ANALYTICA CHIMICA ACTA
·
2024
·
IF 5.7
Linbin Zheng,Meng Li,Zhouyu Jiang,Junyan Fan,Zengbo Fang,Jihuai Zheng,Yan Cui
Background The increased production and use of chiral pesticides will enhance their exposure in the environment. Chiral pesticides typically exhibit varied biological effects among these enantiomers. Therefore, it is very essential to develop and validate chiral analytical methods to investigate their potential ecological risks from a stereoselective perspective. Current separation of pesticides enantiomers relies extensively on chiral stationary phases (CSPs), while the development of β-Cyclodextrin derivatives CSPs become the research focus due to their great modifiability and excellent chiral recognition capabilities. Results A novel chiral stationary phase, 3,5-dichlorophenylaminomethyl-6-phenylenediamine-β-cyclodextrin chemically bonded silica gel (MPDCDA), was successfully prepared. Based on that, a stereoselective HPLC-MS/MS method was developed and validated for the determination of tebuconazole enantiomers in Rana nigromaculata tadpoles. After extraction by QuEChERS, the tebuconazole enantiomers were completely separated with the resolutions of 1.63 using the mobile phase of methanol-water (70/30, v/v). Good linearity (r > 0.9990) for both enantiomers over a concentration range of 0.20–500.0 ng/mL was obtained with the accuracy ranged from 6.7 % to 9.3 % and the intra-day and inter-day precisions below 6.2 % at three quality control levels. The proposed method was successfully applied in evaluating the enantioselective bioaccumulation and elimination profiles of tebuconazole in tadpoles. At the tested conditions, there was no significantly enantioselective difference in the bioaccumulation process for S - tebuconazole and R -tebuconazole. However, the elimination process of tebuconazole enantiomers was enantioselective with R -tebuconazole preferentially degraded. Significance This work provided an accurate risk assessment of chiral pesticides to non-target aquatic organisms from a stereoselective perspective. These findings would deepen our understanding of the potential ecological risks of chiral pesticides on aquatic organisms and provide scientific support for the protection of aquatic organisms and their ecological environments, as well as sustainable development.
研究领域:
分析化学
·
环境科学
·
生态毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2017
·
IF 4.162
Xiu-Xiu Dong,Li-Peng Yuan,Yi-Xin Liu,Min-Fu Wu,Bo Liu,Yuan-Ming Sun,Yu-Dong Shen,Zhen-Lin Xu
Progesterone (P4) is a kind of hormone that can cause neuropathic disturbances in humans when the concentration overpasses a certain degree. In this work, an electrochemical immunosensor capable of detecting P4 sensitively and selectively was developed. Thionine-graphene oxide (Thi-GO) composites with excellent biocompatibility were synthesized and coated to a clear glassy carbon electrode. P4 coating antigen (P4-OVA) was immobilized to the electrode, then sample as well as biotinylated antibody (biotin-P4 Ab) were added. The free P4 can compete with P4-OVA for binding to biotin-P4 Ab. After the further addition of streptavidin-HRP, H 2 O 2 was introduced to develop electrical signal for quantitative determination of P4. After careful optimization of assay conditions, the proposed immunosensor showed a linear range from 0.02 to 20ngmL −1 for P4 in milk samples. The averaged recoveries from spiked samples ranged from 84.0% to 102.0%, which correlated well with standard HPLC-MS/MS. The biosensor also showed good specificity, reproducibility and stability, indicating its potential application in monitoring of P4 in a simple and low cost manner.
研究领域:
分析化学
·
生物传感器
·
电化学
·
纳米材料
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD SCIENCE
·
2020
·Vol. 85
·期 3
·696-706
·
IF 2.479
Meilun Shen,Kang Liu,Yefei Liang,Guangxin Liu,Jie Sang,Cuiqin Li
The aim of this study was to extract and purify anthocyanins from Lycium ruthenicum Murr. and evaluate their tyrosinase inhibitory activity. Response surface methodology was devoted to optimize enzyme-assisted extraction of anthocyanins from L. ruthenicum dried fruits. Extraction at 38 °C for 37 min using water-containing pectinase (52.04 mg/100 g dried fruit) rendered an anthocyanin extraction yield of 19.51 ± 0.21 mg/g. The purified anthocyanins were separated from the extract by macroporous resin XDA-6. Antioxidant tests in vitro suggested that the extract and the purified anthocyanins exhibited a potent 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging capacity, 2,2-azino-bis-3-ethylbenzothiazoline-6-sulfonic acid (ABTS) radical scavenging capacity, hydroxyl radical scavenging capacity, superoxide radical scavenging capacity, and total reducing power. Thirteen anthocyanins from L. ruthenicum dried fruits were analyzed by HPLC-MS. Moreover, the purified anthocyanins had inhibitory effect on tyrosinase monophenolase (IC 50 = 1.483 ± 0.058 mg/mL), and the type of inhibition was competitive inhibition ( K i = 39.83 ± 1.4 mg/mL). The maximum inhibitory activity of the purified anthocyanins (3.00 mg/mL) on tyrosinase diphenolase was 42.16 ± 0.77%, and the type of inhibition was anticompetitive inhibition ( K is = 2.387 ± 0.10 mg/mL). Practical Application The anthocyanins from L. ruthenicum dried fruits can be used as tyrosinase inhibitors in medicine, cosmetics, and food preservation industries.
研究领域:
药理学
·
食品科学
·
生物化学
·
植物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Catalysis Science & Technology
·
2022
·Vol. 13
·期 2
·504-515
·
IF 6.177
Baiyu Liu,Xuefeng Hu,Junhan Yang,Chen Yang,Yao Huang
In this work, direct Z-scheme BiOBr/CuI heterojunctions are successfully synthesized using a simple solvothermal method for the first time. The photocatalytic activity of the BiOBr/CuI composite catalysts is evaluated by the degradation of phenol under visible light. The photocatalytic performance of all the composites is higher than that of the pure components. BiOBr/CuI-1 : 0.8 shows the best photocatalytic performance, which could remove 98.4% phenol in 150 minutes, almost 4.35 and 8.63 times as high as that of pure BiOBr and CuI, respectively. Assisted by XPS, the charge transfer of the composites is investigated. The good photocatalytic performance of the composites is attributed to the Z-scheme charge transfer between BiOBr and CuI. Moreover, the main active species in this system are proved by free radical quenching experiments and EPR, and a possible degradation mechanism is proposed. The degradation products of phenol are analyzed by HPLC-MS and the possible degradation paths are proposed.
研究领域:
材料科学
·
环境科学
·
化学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Qi Zhou,Lihong Wang,Canping Pan,Congcong Yu,Jin Hua,Tao Lan
Considering the matrix characteristics of honeysuckle and chrysanthemum, a comprehensive and systematic extraction and purification processes study for pesticide residue analysis in these two Traditional Chinese Medicine (TCM) were conducted based on a nanomaterial-modified QuEChERS method. For honeysuckle, a combination of 60 mg FeN-MWCNTs and 60 mg PSA provided the best purification effect. For chrysanthemum, 70 mg GCB and 30 mg PSA achieved the optimal results. Our initial exploration into the purification mechanism of the nanomaterials revealed that micropores and smaller mesopores in the adsorbents play a crucial role, while amino groups primarily govern the adsorption process, with matrix impurities adhering to the surface of the nano-adsorbents. The limit of quantification (LOQ) for honeysuckle in this method ranged from 0.12 to 18.86 µg/kg, with recovery rates between 60.1 % and 128.6 %, and relative standard deviations (RSD) less than 12 %. For chrysanthemum, the LOQ was between 0.10 and 8.56 µg/kg, and the recovery rates for 27 pesticides were in the range of 61.6 % to 118.9 %. Applying this method, 105 honeysuckle and 111 chrysanthemum market samples were analyzed, detecting five pesticides in 18 honeysuckle and 12 chrysanthemum samples respectively. This study offers a targeted strategy for the development of analytical methods for trace substances in complex matrices.
研究领域:
分析化学
·
中药学
·
环境科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2026
·
IF 10.6
Fenghong Wei,Pei Wang,Junjun Hu,Yanping Zheng,Xiaojia Huang
Sample preparation is critical in developing a sensitive and accurate method for the monitoring of ultrashort- to long-chain perfluorocarboxylic acids (PFCAs) in complex samples. However, it remains a formidable challenge in the simultaneous and efficient extraction of ultrashort- to long-chain PFCAs (U-L@PFCAs) due to their significantly different polarity. In this connection, the electric field-assisted microextraction (EFAM) was introduced for the first time to efficiently co-extract ultrashort- to long-chain species. According to the chemical properties of the studied U-L@PFCAs, a new microelectrode based on a monolithic adsorbent (MEMA) was tailored using diallylamine and 1,1,1,3,3,3-hexafluoroisopropyl acrylate as dual monomers and employed as the microelectrode of EFAM. Results disclosed that the application of opposite directions and different intensities of electric field at adsorption and desorption stages enhanced the increase of extraction efficiencies by 78.6–131% in comparison with the omission of electric field. In addition, the adsorption characteristics, behavior, and mechanism of MEMA@EFAM towards the investigated U-L@PFCAs were explored. Under the selected microextraction conditions, a sensitive and reliable method based on an isotope internal standard calibration curve technique for monitoring ultra-trace U-L@PFCAs in various environmental water and human urine samples was established by combining MEMA@EFAM with HPLC-MS/MS detection. Low detection limits of 0.13–1.4 ng/L and superior precision (RSDs varied from 2.8% to 9.1%) were achieved with minimum background interference. The present study provides a highly competitive alternative for the broad-spectrum monitoring of PFCAs.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Zongkai Li,Xiaoqing Wang,Qianqian Wang,Zhi Li,Qiuhua Wu,Chun Wang
Endocrine-disrupting bisphenols as endocrine disrupting chemicals present significant risks to the human endocrine system. Developing accurate and highly sensitive methods for detecting trace levels of bisphenols in food is crucial to ensure food safety and prevent health risks. Herein, a hydroxyl-functionalized covalent organic framework (TD-COF) was synthesized using 4,4′,4′'-triaminotriphenylmethane and 3,3′-dihydroxy-[1,1′-biphenyl]-4,4′-dicarbaldehyde as monomer. TD-COF demonstrates superior adsorption ability for bisphenols compared with hydroxyl-free COF, which can be primarily attributed to the presence of hydrogen bonding and π-π interactions. By combining high performance liquid chromatography-mass spectrometry and solid phase extraction technology based on TD-COF, a method for analyzing four bisphenols in river water and chicken was established. Under optimal conditions, the method exhibits a low detection limit (river water: 0.03-0.15 ng mL -1 , chicken: 1.4-3.5 ng g -1 ), satisfactory spiked recovery (river water: 87.0-107%, chicken: 88.5-105 %) and good relative standard deviations (river water: 4.5-6.5%, chicken: 4.0-5.7%).
✓ 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）