JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2011
·
IF 2.971
Jianian Chen,Huijuan He,Shaoshun Li,Qi Shen
The aim of this study is to develop a simple and applicable HPLC method for the detection of vincristine in rat plasma after administration of poly(lactic- co -glycolic acid)–poly(ethylene glycol) (PLGA–PEG) nanoparticles loaded with vincristine sulfate (VCR). Vincristine was extracted from rat plasma and vinblastine sulfate was chosen as the internal standard (IS). Chromatographic separation of VCR and IS was achieved by a Dikma Dimonsil C 18 column (200 mm × 4.6 mm) with the mobile phase consisting of 0.02 M sodium dihydrogen phosphate–methanol (36:64, v/v, pH = 4.7) at a flow rate of 1.0 mL/min. The ultraviolet detection wavelength was set at 276 nm. The calibration curve was linear over a concentration range of 0.05–5.0 μg/mL. The intra-day and inter-day accuracy for three quality controls (QC) samples was 93.48–107.74% and 92.61–96.58%, respectively; the precision was less than 9%. The average method recoveries for vincristine from spiked plasma at all QC levels were over 83%; and extraction recoveries were between 66 and 70%. Vincristine was stable in rat plasma for one month at −80 °C, for 8 h at room temperature , as well as during three freeze–thaw cycles. This HPLC method was applied successfully to the pharmacokinetic study of vincristine in rats after a single intravenous injection of VCR in physiological saline (F-VCR) solution, VCR-loaded PLGA–mPEG nanoparticles with (NP1) and PLGA–PEG–folate nanoparticles (NP2) suspension, respectively. There were significant differences in main pharmacokinetic parameters between F-VCR and the nanoparticles. Both kinds of VCR-loaded nanoparticles displayed improved pharmacokinetic profiles.
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JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Dongqin Tan,Yue Wang,Haocheng Fan,Jing Jin,Xiaoli Sun,Dhanjai,Degao Wang
Magnetic surface imprinted polymer microspheres (Fe 3 O 4 @MIPs) were successfully synthesized via Pickering emulsion polymerization, utilizing N-Methylphenethylamine as a surrogate template for amphetamine-type drugs. Fe 3 O 4 @MIPs not only possessed excellent dispersibility and enough magnetic properties in aqueous solutions, but also displayed good selectivity towards six amphetamines, with an imprinting factor ranging from 1.8 to 2.6. The adsorption kinetics closely aligned with the pseudo-second-order model, and the adsorption efficiency exceeds 80 % for each amphetamine at equilibrium. Fe 3 O 4 @MIPs were then employed as the efficient adsorbents for the extraction of amphetamine drugs. Extraction parameters, including sample pH, the mass of adsorbent, and the type and volume of eluting solvent, were carefully optimized. In combination with the high performance liquid chromatography tandem triple quadrupole mass spectrometry (HPLC-MS/MS), a selective magnetic solid-phase extraction (MISPE) method utilizing Fe 3 O 4 @MIPs was developed for the detection of six amphetamines in water samples. The limits of detection and limits of quantitation were determined to be 5.2∼23 ng L −1 and 17∼77 ng L −1 , respectively. Recoveries for the six target drugs from lake water and sewage samples fell within the range of 87.2∼110 %. Additionally, the MISPE-HPLC-MS/MS method exhibited excellent repeatability, with a precision below 8.5 % at two spiking levels. The prepared Fe 3 O 4 @MIPs possessed the advantages of high selectivity, straightforward preparation, facile separation and good reusability, and was highly suitable for the efficient extraction of amphetamine-type substances in complex environmental water.
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2025
·
IF 4.6
Wenjing Liu,Guangjie Wu,Liping Wang,Jiaying Zhao,Renrong Liu
Immunoaffinity column (IAC) cleanup, coupled with high performance liquid chromatography (HPLC) analysis, is one of the most reliable methods for aflatoxin B1 (AFB1) analysis. However, real-time monitoring of the IAC capacity remains unachievable in IAC-HPLC analysis, compromising the reliability of AFB₁ quantification. Two artificial structural analogues of aflatoxin (AFB1-OH and AFB2-OH) were synthesized as potential markers for IAC capacity monitoring. Competitive ELISA and recovery experiments demonstrated that AFB2-OH was more suitable as a marker. When AFB2-OH was used for real-time monitoring of the capacity of the IAC in AFB1 determination by HPLC, the recovery of AFB1 exceeded 95 %. The limit of detection (LOD) and the limit of quantification (LOQ) for AFB1 were determined to be 0.14 ng/mL and 0.46 ng/mL, respectively. The method also exhibited good precision and accuracy. In spiked recovery experiments of four grains, the recovery of AFB1 ranged from 85.16 % to 107.05 % with relative standard deviations of 0.89 %-4.98 %. More importantly, due to the addition of AFB2-OH, the capacity of the IAC was monitored in real-time, ensuring the reliability of AFB1 determination results.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2025
·
IF 2.8
Jing Lin,Dan Li,Peiyuan Luo,Laisheng Li
A bis (3,5-dichlorophenylureido)-β-cyclodextrin stationary phase (CUCDP) was prepared and characterized. It had strong chiral separation abilities for antihistamines ( R s = 1.61–2.58) in isocratic elution, including chlorpheniramine maleate, bromopheniramine maleate, promethazine hydrochloride and trimeprazine tartrate. Based on CUCDP, a new HPLC method for simultaneous separation and determination of the above eight antihistamine enantiomers ( R s = 1.58–1.92) in human plasma by gradient elution was established. The optimized conditions were as follows: a simple sample pretreatment with acetonitrile (ACN) to precipitate protein, a gradient elution of 0.5 % triethylammonium acetate (TEAA, pH = 4.0)-ACN as the mobile phase at a flow rate of 0.5 mL/min, column temperature at 20 °C, a photo-diode array detector (PDA) at 260 nm, and the sampling volume of 10 μL. The good linear relationships for all enantiomers were observed in the concetration range of 0.25–10.0 μg/mL ( R 2 = 0.9986–0.9993). The average recoveries were 84.80 %–103.30 % with the RSDs of 1.24 %–2.26 % ( n = 5). The limits of detection (LODs) and limits of quantification (LOQs) were 0.015–0.05 μg/mL and 0.05–0.15 μg/mL, respectively. At present, the reported cyclodextrin-based CSPs had not such separation ability for antihistamines by HPLC. However, the new CUCDP exhibited high chiral selectivity for antihistamines, which was mainly related to the introduction of bis phenylureido group into the rim of cyclodextrin, and the strengthening of hydrogen bonding, π–π stacking and inclusion between CUCDP and analytes. This method could save analysis time, reduce solvent consumption, and improve efficiency at low cost.
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高影响因子
CHIRALITY
·
2024
·Vol. 36
·期 5
·e23672
·
IF 2.8
Chen Chen,Yangfeng Peng,Yongming Wei,Mengyuan Liu,Yu Wang,Siqi Xiong,Huiyi Li,Quan He
Hydroxychloroquine (HCQ), 2-([4-([7-Chloro-4-quinolyl]amino)pentyl]ethylamino)ethanol, exhibited significant biological activity, while its side effects cannot be overlooked. The RP-HPLC enantio-separation was investigated for cost-effective and convenient optical purity analysis of HCQ. The thermodynamic resolution of Rac-HCQ, driven by enthalpy and entropy, was achieved on the C18 column using Carboxymethyl-β-cyclodextrin (CM-β-CD) as the chiral mobile phase agent (CMPA). The effects of C CM-β-CD , pH, and triethylamine (TEA) V% on the enantio-separation process were explored. Under the optimum conditions at 24°C, the retention times for the two enantiomers were t R 1 = 29.39 min $$ {t}_{R1}=29.39\ \min $$ and t R 2 = 32.42 min $$ {t}_{R2}=32.42\ \min $$ , resulting in R s = 1.87 $$ {R}_s=1.87 $$ . The resolution via diastereomeric salt formation of Rac-HCQ was developed to obtain the active pharmaceutical ingredient of single enantiomer S-HCQ. Di-p-Anisoyl-L-Tartaric Acid (L-DATA) was proved effective as the resolution agent for Rac-HCQ. Surprisingly, it was found that refluxing time was a key fact affecting the resolution efficiency, which meant the kinetic dominate during the process of the resolution. Four factors—solvent volume, refluxing time, filtration temperature, and molar ratio—were optimized using the single-factor method and the response surface method. Two cubic models were established, and the reliability was subsequently verified. Under the optimal conditions, the less soluble salt of 2L-DATA:S-HCQ was obtained with a yield of 96.9% and optical purity of 63.0%. The optical purity of this less soluble salt increases to 99.0% with a yield of 74.2% after three rounds recrystallization.
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Journal of Applied Research on Medicinal and Aromatic Plants
·
2024
·
IF 3.8
Yushu Sui,Liben Pan,Nan Yang,Xiaorui Guo,Zhonghua Tang
In the present study, developed a dependable HPLC technique to quantify asarinin and sesamin in Asarum heterotropoides Fr. Schmidt var. mandshuricum (Maxim.) Kitag. The optimal conditions for the ultrasonic-assisted extraction were determined by conducting single-factor experiment, Plackett-Burman design experiment, and Box-Behnken response surface method . Based on actual operation factors and analysis, the optimal extraction parameters were methanol volume fraction of 80% (v/v), liquid-to-material ratio of 10:1 (mL/g), ultrasonic time of 40 min, ultrasonic temperature of 51°C, and ultrasonic power of 300 W. When subjected to these conditions, the average asarinin and sesamin content were found to be 13.40 mg/g and 2.39 mg/g, respectively, with a relative error of 1.04% and 3.46%, which was consistent with the theoretical value. This study can offer a theoretical reference for the extraction of asarinin and sesamin in Asarum .
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JOURNAL OF SOLID STATE CHEMISTRY
·
2021
·
IF 3.498
FuKai Li,Min Wang,Jian Zhou,MengRui Yang,TongTong Wang
A novel magnetically and efficiently multifunctional boronic acid (BA) -functionalized core-shell nanohybrid (Fe 3 O 4 @SiO 2 @BA) was prepared for capture and separation of cis -diol-flavonoids. The morphology and physicochemical properties of resultant nanoparticles were systematically characterized via several techniques, and the results confirmed that the target nanohybrids were successfully functionalized and modified. Meanwhile, two flavonoids (quercetin and luteolin) were selected to investigate the selective capture of the Fe 3 O 4 @SiO 2 @BA in procedure of magnetic solid phase extraction (MSPE). The main parameters influencing the adsorption and elution conditions were systematically investigated and optimized. Furthermore, the adsorption kinetic models were adopted to elucidate the adsorption process , indicating that the pseudo-second-order model was suitable to explain the adsorption kinetics. Under the optimum conditions, the MSPE-HPLC-MS/MS approach was established with a wide linear dynamic range and good linearity (R 2 > 0.999), low limits of detection (0.0096–0.033 μg L −1 ) and satisfactory recoveries (91–107.6%). The proposed analytical method was successfully applicated by determining the content of target flavonoids in food samples (apple and onion). Accordingly, the prepared nanohybrid could serve as an efficient, rapid and economical potential adsorbent for extracting cis -diol-flavonoids in complex food samples.
研究领域:
纳米技术
·
分析化学
·
食品科学
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高影响因子
FOOD RESEARCH INTERNATIONAL
·
2015
·
IF 2.818
Lu Zhang,Zong-cai Tu,Hui Wang,Zhi-feng Fu,Qing-hui Wen,Hai-xia Chang,Xiao-qin Huang
This study aimed to compare the extraction efficiency of dynamic high pressure microfluidization-assisted extraction (DHPMAE) and other commonly used extraction methods on the antioxidant activities (AAs) of sweet potato leaves ( Ipomoea batatas L., SPL), and to identify the antioxidant compounds by HPLC-QTOF-MS 2 . Two highly consumed commercial varieties, orange-fleshed and cream-fleshed sweet potato leaves (OFL and CFL), were taken as materials. OFL was evidenced to be a better antioxidants resource than CFL due to higher polyphenols and AAs. DHPMAE had the best extraction efficiency on total phenolics and total flavonoids , with the values in OFL extract at 16.35 mg GAE/g DM and 16.51 mg RE/g DM, respectively. DHPMAE extract also exhibited the strongest DPPH· and ABTS· + scavenging ability, chelating ability and reducing power. Multiple regression analysis revealed that polyphenols played an important contribution to the AAs of SPL extracts. After successive fractionation of DHPMAE extract by chloroform, ethyl acetate, and n -butanol, the ethyl acetate fraction showed the highest total phenolic (569.38 mg GAE/g Extract) and total flavonoid (43.15 mg RE/g Extract) content, as well as the highest AAs. HPLC-QTOF-MS 2 analysis of the ethyl acetate fraction resulted in identifying 37 compounds including 20 phenolic acids , 12 flavonoids, 3 organic acids, 1 nucleoside and 1 ester, and 20 of them were firstly detected in SPL. Caffeoylquinic acid derivatives and flavonoids were the most abundant antioxidant compounds. The presented results suggested that DHPM might be a promising assisted technology in extracting polyphenols from plants, and SPL could be utilized for the development of functional food.
研究领域:
食品科学
·
植物化学
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JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY
·
2015
·Vol. 15
·期 12
·9578-9584
·
IF 1.556
Qiu Xiu-Zhen,Liang Yong,Guo Hui-Shi,Wang Xiao-Bing,Lin Chuang-Xin
A novel molecularly imprinted polymer (MIP) was synthesized using halloysite nanotubes (HNT) as matrix, β-cyclodextrin (β-CD) and methyl propyl acid (MAA) as functional monomers, and 2,4,6-TCP as template molecule by graft copolymerization. Infrared spectroscopy
and transmission electron microscopy (TEM) were used to characterize the as-synthesized imprinted polymer. The selective recognizability of the MIP towards four phenolic analogs were determined and the recognition coefficients for 2,4,6-TCP, 2,6-DCP, 4-CP and phenol were found to be 2.17,
1.85, 2.02 and 1.36, respectively. Using as the packing material of solid-phase extraction, the imprinted polymer has been applied to on-line extraction of the four phenolic compounds in environmental water. The corresponding analytical methods to determine these four phenolic compounds have
been developed. Good linear relationships were obtained over the range of 0.05∼5.0 mg ·L−1. The average recoveries for spiked samples were in the range of 74.8∼97.2%, and the detection limits for 2,4,6-TCP, 2,6-DCP, p-chlorophenol, phenol were 0.19, 0.20,
0.75, 0.73 mg · L−1, respectively. The method is rapid, accurate and high selectivity. It was feasible for the determination of trace level phenolic compounds in environmental samples.
研究领域:
分析化学
·
环境科学
·
材料科学
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高影响因子
Journal of the Iranian Chemical Society
·
2017
·Vol. 14
·期 9
·2017-2022
·
IF 1.407
Qin Xingxiu,Bakheet Almojtaba AbdAlkhalig Ahmed,Zhu Xiashi
Fe 3 O 4 @ionic liquids β-cyclodextrin polymer(Fe 3 O 4 @mono-6-deoxy-6-(1-ethyl-imidazolium)-β-cyclodextrin iodide polymer, Fe 3 O 4 @ILs-β-CDCP) was prepared. Magnetic solid phase extraction coupled with high-performance liquid chromatography for the separation/analysis of congo red (CR) in water and drysaltery was established. Fe 3 O 4 @ILs-β-CDCP showed a higher adsorption capacity toward CR. CR was adsorbed rapidly by Fe 3 O 4 @ILs-β-CDCP (adsorption efficiency: 95%) and eluted by ethanol (elution efficiency: 96%) at room temperature. Under the optimal conditions, preconcentration factor of the proposed method was 20-fold. The linear range, correlation coefficient ( R
2 ), detection limit (DL) and relative standard deviation were found to be 0.005–100.00 µg mL −1 , 0.9910, 1.8 g L −1 and 0.61% ( n = 3, c = 5.00 µg mL −1 ), respectively. The adsorption mechanism of CR on Fe 3 O 4 @ILs-β-CDCP was studied through the FTIR analysis. The accuracy of the developed method was confirmed by spiking city water, lake water, pond water and drysaltery. Fe 3 O 4 @ILs-β-CDCP can be used repeatedly for 10 times. This proposed method had been successfully applied to the determination of CR in real samples.
研究领域:
分析化学
·
环境科学
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MICROCHIMICA ACTA
·
2011
·Vol. 175
·期 3
·341-346
·
IF 2.578
Jiang Xinyu,Zhang Hui,Chen Xiaoqing
We report on the determination of bisphenol A and 2-naphthol in water samples using ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction combined with HPLC. Parameters governing the extraction efficiency (disperser solvent, volume of extraction and disperser solvent, pH, temperature, extraction time) were optimized and resulted in enrichment factors of 112 for bisphenol A and of 186 for 2-naphthol. The calibration curve was linear with correlation coefficients of 0.9995 and 0.9998, respectively, in the concentration range from 1.5 to 200 ng mL −1 . The relative standard deviations are 2.3% and 4.1% (for n = 5), the limits of detection are 0.58 and 0.86 ng mL −1 , and relative recoveries in tap, lake and river water samples range between 100.1 and 108.1%, 99.4 and 106.2%, and 97.1 and 103.8%, respectively.
IL-CIA-DLLME has a high enrichment factor (112, 186), acceptable relative recovery (97.1%–108.1%), good repeatability (2.3%, 4.1%) and a wide linear range(1.5–200 ng mL −1 ) for the determination of bisphenol A and 2-naphthol.
研究领域:
分析化学
·
环境科学
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JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2016
·
IF 0.669
Yu Wang,Jing Yang,Yanfang Guo,Haipeng Wang,Yalan Liu,Huiming Huang,Baogang Xie
The determination of alendronate (ALE) in biofluids using a low-cost instrument is potentially useful in preclinical pharmacokinetic studies. This study developed and validated a high-performance liquid chromatography with ultraviolet method for ALE determination in rat plasma using precolumn derivatization with phenyl isothiocyanate (PITC). Inhibiting compounds in the samples were first eliminated using solid-phase extraction. ALE in the sample was subsequently allowed to react with PITC to form a phenylthiocarbamoyl derivative for further analysis. The assay was linear within the concentration range of 0.29–25.0 µg/mL. The precision and accuracy were less than 3.9% and 98.0 ± 3.9%, respectively. The limits of detection and quantification were 0.08 and 0.20 µg/mL, respectively. The method was successfully used to evaluate the pharmacokinetic parameters of ALE in rats following a single oral administration (30.0 mg/kg). The results show that the peak plasma ALE concentration is 0.69 ± 0.18 µg/mL. The area under the plasma concentration–time curve value of ALE was 2.14 ± 0.68 µg/mL hr. This method can suitably evaluate the bioavailabilities of different ALE dosage forms in preclinical pharmacokinetic studies.
研究领域:
药物分析
·
临床药理学
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高影响因子
危险品化学品经营许可证（带存储）