International Journal of Analytical Chemistry
·
2026
·Vol. 2026
·期 1
·6094234
·
IF 2.8
Amna Naz,Muhammad Farooq,Muhammad Sarfraz,Ahsanullah Unar,Rouheena Shakir,Hafiz Arfat Idrees,Nadia Anwar
Oleanolic acid (OL) and genistein (GN) are bioactive compounds known for their anti-inflammatory, antioxidant, antiviral, cardioprotective, and anticancer properties. Their synergistic therapeutic potential motivated the development of a hybrid nanoformulation, comprising GN nanoparticles incorporated into an OL-loaded liposomal system named GOL. The formulation was extensively characterized for particle size, polydispersity index, zeta potential, entrapment efficiency, and pharmacokinetic behavior, demonstrating its suitability for co-delivery of both drugs. To accurately quantify OL and GN in the GOL system, a robust HPLC-UV method was developed and validated. Simultaneous determination was challenging due to distinct chemical and spectral properties; OL showed λmax at 210–215 nm, while GN had λmax at 215, 270, and 336 nm. Optimization using a Box–Behnken design yielded a method using a C18 column with a methanol–acetonitrile–water–tetrahydrofuran (60:20:8:12, v/v) mobile phase and detection at 230 nm. Retention times were 4.8 and 9.9 min for OL and GN. Plasma samples were processed via simple protein precipitation. The method met ICH validation criteria for sensitivity, selectivity, accuracy, precision, robustness, and stability. Finally, the developed method was successfully applied to analyze both drugs from the GOL nanoformulation in both biological fluids and polymeric matrices, enabling a reliable assessment of drug content and stability.
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ANALYTICA CHIMICA ACTA
·
2024
·
IF 5.7
Jiankun Cao,Mingwei Wang,Yehong Han,Mingyu Wang,Hongyuan Yan
Background The detection of disease biomarkers in biological samples plays an important role in early diagnosis and treatment of carcinoid tumor. However, due to the complexity of biological samples and the extremely low concentration of disease biomarkers, sample pretreatment is still the bottleneck of achieving accurate quantitative determination . In this work, new hydrophilic molecularly imprinted resin-hexagonal boron nitride (HMIR-h-BN) composites were developed and used as a new solid phase extraction (SPE) adsorbent for selective detection of 5-hydroxyindoleacetic acid (5-HIAA), a biomarker of carcinoid tumor, in urine. Results Twenty-two types of HMIR-h-BN were successfully synthesized through growing hydrophilic molecularly imprinted resin on surface of activated two-dimensional h-BN nanosheets , and preparation parameters affecting the adsorption performance of HMIR-h-BN were investigated and optimized through adsorption experiments. HMIR-h-BN #19 (the ratio of resorcinol to hexamethylenetetramine : 6:3; the dosage of h-BN: 300 mg; the dosage of dummy template: 0.12 mmol; the imprinting time: 4 h) has demonstrated to be the optimal material for efficient separation and extraction of 5-HIAA. Combined with HPLC-UV, the limit of detection and the limit of quantification of 5-HIAA in real urine samples were 9.4 ng mL −1 and 31.3 ng mL −1 , respectively, the coefficient of determination (R 2 ) was 0.9996 in the linear range of 0.1–300 μg mL −1 and the relative recoveries ranged from 86.9 % to 97.7 % with RSD ≤5.1 %. Moreover, after being processed by HMIR-h-BN-SPE, there are no interferences from other peaks at the peak position of 5-HIAA. Significance The HMIR-h-BN composite has been demonstrated to be capable of selective extraction of 5-HIAA from urine samples and have a significant purification effect. Based on the established HMIR-h-BN-SPE-HPLC-UV method, accurate quantitative determination of 5-HIAA in urine samples was achieved, which is expected to be applied in the early diagnostic of carcinoid tumor.
研究领域:
分析化学
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生物医学工程
·
临床化学
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材料科学
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Frontiers in Nutrition
·
2025
·
IF 5.1
Xiaojie Zhang,Lan Yang,Haifei Lian,Zixuan Xu,Zichen Yun,Xiaohui Xu,Shixiong Liu,Qifei Luo,Majigsuren Zolzaya,Dacheng Liu
Background: Composite yeast culture (CYC) serves as an important functional feed additive. The content of its active ingredient, α-mannan, directly affects product quality and efficacy. However, due to the complex matrix of CYC, establishing a highly specific and accurate quantitative method for α-mannan remains a challenge.Methods: This study aimes to establish an analytical method based on enzymatic hydrolysis combined with high-performance liquid chromatography equipped with an ultraviolet detector (HPLC-UV) for the quantification of α-mannan in CYC. The method involved the specific enzymatic hydrolysis of α-mannan in the sample using α-mannosidase, followed by the release of mannose, which was then derivatized with 1-phenyl-3-methyl-5-pyrazolone (PMP) and analyzed by HPLC-UV. The actual content of α-mannan was calculated using a formula.Results: Method validation results showed that mannose exhibited good linearity within the concentration range of 0.5–400 μg/mL, with a correlation coefficient of 0.99998. The limit of detection (LOD) and limit of quantification (LOQ) were 0.063 mg/L and 0.208 mg/L, respectively. The average recovery rate was 88.020%−94.204%, with a relative standard deviation (RSD) ranging from 0.702% to 2.259%, indicating that the method has high accuracy and good precision.Conclusion: This study successfully established an efficient and reliable HPLC-UV detection method suitable for the specific quantitative analysis of α-mannan in CYC. The method exhibited good reproducibility and operational feasibility, providing robust technical support for quality control of CYC products and related functional component research.
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MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 11
·1-9
·
IF 5.479
Hou Xingyu,Huang Wei,Tong Yukui,Tian Miaomiao
The authors describe boronate-modified hollow dummy template imprinted polymers (B-hDIPs) for selective and sensitive extraction of the catecholamines norepinephrine (NE), epinephrine (E), and dopamine (DA) from urine samples prior to their detection by HPLC with UV detector. The B-hDIPs were prepared by using (a) nano-TiO 2 as the sacrificial support, (b) 3-carboxyphenylboronic acid (CPBA) as the boronate-affinity functional monomer, and (c) catechol which acts as dummy template. The nano-TiO 2 can be etched off by using hydrofluoric acid to form the hollow imprint. The main advantages of using such hollow polymers arise from their controllable hole structure which favors template removal and fast mass transfer. The B-hDIPs material was characterized by FT-IR, transmission electron microscope, dynamic light scattering, X-ray photoelectron spectrum, and thermal gravimetric analysis. The effects of imprinting conditions, sample pH, sample flow rate, adsorbent amount, selectivity and competitive capacities were investigated. Under optimal conditions, the limits of detection for the catecholamines are in the range from 15 to 47 ng mL −1 . The method was successfully applied to their determination of NE, E, and DA in spiked urine, with recoveries ranging from 63.4 to 106.2%.
Schematic presentation of boronate-modified hollow dummy template imprinted polymers as an adsorbent to extraction of the catecholamines (norepinephrine, epinephrine, and dopamine) from urine samples prior to their detection by HPLC-UV.
研究领域:
分析化学
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医学检测
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材料科学
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Food Analytical Methods
·
2023
·Vol. 16
·期 4
·689-698
·
IF 2.9
Chu Qiqi,Wu Xinze,Chen Huaixia,Dang Xueping,Liu Xiaolan
A Cu 7 Zn 2 cluster functionalized copolymer monolithic column was prepared and applied as the adsorbent of pipette tip micro-solid phase microextraction of eight phthalate esters (PAEs). The physical morphology, chemical composition, thermal stability, and specific surface area of the monolithic column were characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, thermogravimetric analysis, and N 2 adsorption and desorption experiment. Cu 7 Zn 2 cluster acted as the adsorption site effectively improved the adsorption selectivity and capacity of the copolymer monolith for PAEs. The adsorption mechanism of Cu 7 Zn 2 copolymer monolith for 8 PAEs was deduced to be mainly the H-bond interaction. And, the chemical doping and copolymerization of Cu 7 Zn 2 cluster made the composite monolithic column more stable with a long service life. Under the optimized extraction conditions, a micro-solid phase extraction-high performance liquid chromatography method with ultraviolet detector (μ-SPE-HPLC-UV) was developed for the determination of 8 PAEs in edible oil. Wide linear ranges of 0.5–1000 μg/kg with correlation coefficients ( R 2 ) above 0.996 were obtained. The limits of detection (LODs) were in the range of 0.1–0.9 μg/kg. The proposed method was applied for the detection of 8 PAEs in edible oil with satisfactory recoveries between 83.5~100.2%, and the relative standard deviations were less than 8.1%. The results indicated that the Cu 7 Zn 2 functionalized copolymerized monolithic column was an ideal enrichment medium for the detection of PAEs in complex samples.
研究领域:
分析化学
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环境科学
·
材料科学
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ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2016
·Vol. 23
·期 19
·19409-19416
·
IF 2.76
Peng Guilong,He Qiang,Lu Ying,Mmereki Daniel,Zhong Zhihui
A simple method based on dispersive solid-phase extraction (DSPE) and dispersive liquid–liquid microextraction method based on solidification of floating organic droplets (DLLME-SFO) was developed for the extraction of chlorpyrifos (CP), chlorpyrifos-methyl (CPM), and their main degradation product 3,5,6-trichloro-2-pyridinol (TCP) in tomato and cucumber samples. The determination was carried out by high performance liquid chromatography with ultraviolet detection (HPLC-UV). In the DSPE-DLLME-SFO, the analytes were first extracted with acetone. The clean-up of the extract by DSPE was carried out by directly adding activated carbon sorbent into the extract solution, followed by shaking and filtration. Under the optimum conditions, the proposed method was sensitive and showed a good linearity within a range of 2–500 ng/g, with the correlation coefficients ( r ) varying from 0.9991 to 0.9996. The enrichment factors ranged from 127 to 138. The limit of detections (LODs) were in the range of 0.12–0.68 ng/g, and the relative standard deviations (RSDs) for 50 ng/g of each analytes in tomato samples were in the range of 3.25–6.26 % ( n = 5). The proposed method was successfully applied for the extraction and determination of the mentioned analytes residues in tomato and cucumber samples, and satisfactory results were obtained.
研究领域:
食品科学
·
分析化学
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FOOD CHEMISTRY
·
2021
·
IF 7.514
Liye Wang,Jiangxiu Niu,Pengyuan Wei,Yilei Feng,Mingyue Ding,Chaojun He,Yongjie Ma,Yaolei Zhu,Jia Li,Lingli Huang,Xiya Zhang
To reduce matrix interference and realize simultaneous detection of multiple homologous compounds (trimethoprim (TMP), diaveridine (DVD), ormetoprim (OMP), baquiloprim (BQP), and aditoprim (ADP) in pig, cattle, chicken, and fish muscles), an immunomagnetic bead (IMB)-based sample purification pretreatment with HPLC–UV was developed. A broad-spectrum monoclonal antibody (mAb, named 14C6) was prepared and conjugated with carboxylic-acid-functionalized magnetic nanoparticles using the active ester method to obtain IMBs for sample purification. The extraction solvent was optimized based on the extraction efficiency. Good linearity was observed for all the five analytes (10–200 μg/kg) with the LOD and LOQ of 5 and 10 μg/kg, respectively. The mean recoveries ranged from 62.5% to 76.9%, while the coefficient of variation was <12.2%. The IMB method afforded greater sample purification and enrichment than those achieved with the SPE column-based conventional method. Hence, the IMB-based sample purification is a useful tool to determine 2,4-diaminopyrimidine residues in edible animal tissues.
研究领域:
分析化学
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食品安全
·
兽医学
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Natural Product Communications
·
2023
·
IF 1.8
Wenjia Li,Qinggui Lei,Wenqing Li,Guoying Tan,Xingzhong Liu,Zhengming Qian
A high-performance liquid chromatography (HPLC) method for the determination of 4 nucleosides by one reference compound in Chinese cordyceps was developed. The sample of Chinese cordyceps was prepared by ultrasonic extraction with a 0.5% phosphoric acid aqueous solution. The separation of the sample was performed on a CORTECS T3 column (100 mm × 4.6 mm, 2.7 μm) by gradient elution with acetonitrile and water at a flow rate of 1.0 mL/min. The wavelengths were set as 258 nm (0-5 min), 252 nm (5-9.1 min), 258 nm (9.1-10.5 min), 249 nm (10.5-20 min) at which 4 nucleosides exhibited identical ultraviolet absorption. The accuracy, precision, reproducibility, and stability tests of the HPLC method were carried out, and the results indicated that the established HPLC method was suitable for the quantitative analysis of 4 nucleosides in Chinese cordyceps. This approach was compared to the traditional external standard method with 4 nucleoside reference compounds and the relative standard errors of the content determination results by the 2 methods were less than 3.5%. The HPLC method developed for quantitative measurement of 4 nucleosides in Chinese cordyceps is simple, lower cost, and time-saving, which provides a methodology alternative for quality control of Chinese cordyceps.
研究领域:
分析化学
·
药学
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Chun-Ying Xu,Chang-Qing Zhen,Yu-Jing He,Yuan-Yuan Cui,Cheng-Xiong Yang
The abnormal estrogens levels in human body can cause many side effects and diseases, but the quantitative detection of the trace estrogens in complex biological samples still remains great challenge. Here we reported the fabrication of a novel core-shell structured magnetic cyclodextrin microporous organic network (Fe 3 O 4 @CD-MON) for rapid magnetic solid phase extraction (MSPE) of four estrogens in human serum and urine samples prior to HPLC-UV determination. The uniform spherical core-shell Fe 3 O 4 @CD-MONs was successfully regulated by altering the reactive monomers and solvents. The Fe 3 O 4 @CD-MONs owned high specific surface area, good hydrophobicity, large superparamagnetism, and abundant extraction sites for estrogens. Under optimal conditions, the proposed MSPE-HPLC-UV method provided wide linearity range (2.0–400 μg L −1 ), low limits of detection (0.5–1.0 μg L −1 ), large enrichment factors (183–198), less adsorbent consumption (3 mg), short extraction time (3 min), and good stability and reusability (at least 8 cycles). The established method had also been successfully applied to the enrichment and detection of four estrogens in serum and urine samples with a recovery of 88.4–105.1 % and a relative standard deviation of 1.0–5.9 %. This work confirmed the feasibility of solvent and monomer regulation synthesis of Fe 3 O 4 @CD-MON composites, and revealed the great prospects of magnetic CD-MONs for efficient enrichment of trace estrogens in complex biological samples.
研究领域:
分析化学
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材料科学
·
生物医学工程
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2013
·
IF 2.487
Shian Zhong,Yanyue Kong,Ling Zhou,Chengyun Zhou,Xiaona Zhang,Yan Wang
In this study, we developed an efficient conversion process of dihydromyricetin to myricetin from Ampelopsis grossedentata extracts. The content of myricetin increased from 2.38% to 85.57%, demonstrating the successful dehydrogenation of dihydromyricetin. Molecularly imprinted polymers (MIPs) were prepared by surface imprinting method using silica microspheres as the support matrices and myricetin as template. The MIPs were applied for the selective adsorption of myricetin. The chemical structure of the MIPs was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. Static, dynamic and selective adsorption experiments showed that the MIPs exhibited good adsorption ability, rather fast template rebinding kinetics, and appreciate selectivity over structurally related compounds. Accordingly, the MIPs were applied as the selective sorbent in SPE to purify myricetin obtained through dehydrogenation, followed by HPLC-UV analysis. The recoveries of myricetin and dihydromyricetin were 92.7% and 55.6%, respectively. This study demonstrates the feasibility of using the developed MIP-SPE method to purify and enrich myricetin in the natural products.
研究领域:
药学
·
分析化学
·
天然产物化学
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高影响因子
MOLECULES
·
2022
·Vol. 27
·期 18
·6084
·
IF 4.927
Tingting Zhou,Ziwen Deng,Qing Wang,Hui Li,Shun Li,Xuanming Xu,Yusun Zhou,Shukai Sun,Chao Xuan,Qingwu Tian,Limin Lun
In this work, novel selective recognition materials, namely magnetic molecularly imprinted polymers (MMIPs), were prepared. The recognition materials were used as pretreatment materials for magnetic molecularly imprinted solid-phase extraction (MSPE) to achieve the efficient adsorption, selective recognition, and rapid magnetic separation of methotrexate (MTX) in the patients’ plasma. This method was combined with high-performance liquid chromatography–ultraviolet detection (HPLC–UV) to achieve accurate and rapid detection of the plasma MTX concentration, providing a new method for the clinical detection and monitoring of the MTX concentration. The MMIPs for the selective adsorption of MTX were prepared by the sol–gel method. The materials were characterized by transmission electron microscopy, Fourier transform-infrared spectrometry, X-ray diffractometry, and X-ray photoelectron spectrometry. The MTX adsorption properties of the MMIPs were evaluated using static, dynamic, and selective adsorption experiments. On this basis, the extraction conditions were optimized systematically. The adsorption capacity of MMIPs for MTX was 39.56 mgg−1, the imprinting factor was 9.40, and the adsorption equilibrium time was 60 min. The optimal extraction conditions were as follows: the amount of MMIP was 100 mg, the loading time was 120 min, the leachate was 8:2 (v/v) water–methanol, the eluent was 4:1 (v/v) methanol–acetic acid, and the elution time was 60 min. MTX was linear in the range of 0.00005–0.25 mg mL−1, and the detection limit was 12.51 ng mL−1. The accuracy of the MSPE–HPLC–UV method for MTX detection was excellent, and the result was consistent with that of a drug concentration analyzer.Keywords:methotrexate;magnetic molecularly imprinted polymers;magnetic molecularly imprinted solid-phase extraction;high-performance liquid chromatography–ultraviolet detection
研究领域:
医学分析
·
药物检测
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RSC Advances
·
2025
·Vol. 15
·期 46
·38585-38596
·
IF 4.6
Shukai Sun,Yue Zhai,Qingwu Tian,Peng Zhao,Hong Cheng,Deng Pan,Junna Sui,Yusun Zhou,Chao Xuan,Tingting Zhou
Magnetic molecularly imprinted polymers (MMIPs) were synthesized using magnetic Fe3O4@SiO2 as a carrier for the selective recognition and adsorption of doxorubicin (DOX) and epirubicin (EPI) in plasma. Then, the method was combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) to realize rapid and accurate detection of DOX and EPI concentrations in plasma. The structures of the prepared MMIPs were characterized by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, and magnetic saturation. As observed, the prepared MMIPs had a uniform appearance and excellent magnetic properties. Then, the adsorption performance of MMIPs was verified through static, dynamic, and selective adsorption tests. MMIPs were found to have high adsorption capacity (8.36 and 8.19 mg g−1), high selectivity (imprinting factors of 34.83 and 8.03), and rapid adsorption for DOX and EPI, respectively. Next, HPLC-UV was used for quantitative analysis. The prepared method had a good linear relationship (0.0001–0.5 mg mL−1 for DOX and 0.0002–0.5 mg mL−1 for EPI) and low detection limits (0.04613 ng mL−1 for DOX and 0.08969 ng mL−1 for EPI). The combination of magnetic solid-phase extraction and HPLC-UV was a highly specific and sensitive method for determining DOX and EPI concentrations in plasma.
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