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.
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Food Analytical Methods
·
2022
·Vol. 15
·期 9
·2479-2486
·
IF 3.498
Zhang Shengnan,Li Zhibo,Qi Yanxia,Yu Pei,Zhao Qiancheng
The determination of 2-acetyl-1-pyrroline (2-AP), which is an important flavour compound of crustaceans and has a low odour threshold of 0.05 μg/L in water, is still a challenge due to the instability and trace levels of 2-AP in food samples. In this study, 2-AP was trapped by o-phenylenediamine and subsequently purified by the dispersive solid-phase extraction and dispersive liquid–liquid microextraction (DSPE-DLLME) methods for HPLC–UV analysis. The developed method was simple, fast and sensitive for the determination of 2-AP in shrimp. Under the optimized DSPE-DLLME conditions, the developed method exhibited excellent linearity ( R 2 = 0.996) and a low limit of detection (LOD, 1.77 μg/kg) and limit of quantitation (LOQ, 5.33 μg/kg). The recoveries of 2-AP in shrimp ranged from 86.3 to 101.6%. In addition, the developed method was applied to detect 2-AP levels in baked shrimp (ranging from 5.6 to 12.6 μg/kg), indicating that the formation of 2-AP could be observed in thermally treated shrimp depending on heating temperature and time. In summary, the developed method has potential application for the trace determination of 2-AP in shrimp due to its convenience and high sensitivity.
研究领域:
食品科学
·
分析化学
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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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高影响因子
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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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2023
·
IF 3
Hong Yang,Jing Wang,Wenming Cao
Tetramethylpyrazine (TMP) is an important bioactive compound in vinegars, contributing to their health-enhancing attributes. It serves as a crucial benchmark for the assessment of vinegar quality. Unfortunately, inaccuracies have arisen due to incomplete extraction techniques and the use of an inappropriate standard substance. These challenges have significantly curtailed comprehensive exploration into the underlying TMP formation mechanisms, impeding advancements within prevailing benchmarks and methodologies governing vinegar products. To address these challenges, several critical parameters, encompassing pH, solvent type, centrifugal force, extraction times and reference materials were investigated and optimized. The TMP content was determined by adjusting the pH to 9 using a sodium hydroxide solution, followed by extraction with ethyl acetate and subsequent re-extraction of the ethyl acetate layer with 0.2 mol/L HCl. A high-performance liquid chromatography method with an ultraviolet detector (UV) was developed and validated. This method demonstrated superior sensitivity compared to existing methods, with a limit of detection (LOD) of 0.0237 μg/g, limit of quantification (LOQ) of 0.0829 μg/g, method limit of detection (MLOD) of 0.10 μg/g and method limit of quantitation (MLOQ) of 0.25 μg/g. The modified method exhibited excellent linearity for TMP in the range of 0.1–118.4 μg/mL, with a good correlation coefficient (R 2 > 0.999). The recovery rate of TMP in vinegar products ranged from 82.4 to 96.2%. Consequently, the proposed method exhibits substantial promise for systematic inquiry into TMP formation mechanisms and for ensuring consistent quality control during the production of premium-grade vinegars.
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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
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2017
·Vol. 55
·期 6
·662-668
·
IF 0.984
Ma Xiaowei,Feng Fan,Yang Yang,Dang Xueping,Huang Jianlin,Chen Huaixia
Fe3O4@MIL-100 (MIL, Material Institut Lavoisier) core–shell magnetic microspheres were prepared and applied as the sorbent for the magnetic solid phase extraction (MSPE) of N,N-diethyl-m-toluamide (DEET) in baby toilet water for the first time. The synthesized magnetic metal–organic frameworks were characterized by transmission electron microscope, infrared spectroscopy and thermogravimetric analysis. The functionalized magnetic microparticles showed excellent dispersibility in aqueous solution. The MSPE conditions were investigated in detail. Under the optimized conditions, an MSPE–high performance liquid chromatography method for the determination of DEET was developed. The method was linear in the concentration range from 5 to 500 μg L−1 for DEET in baby toilet water and good linearity (r2 > 0.9998) was obtained for the calibration curve. The limit of detection was 1.5 μg L−1. Both the intra-day and inter-day precisions (relative standard deviations) were <3%.
研究领域:
分析化学
·
环境科学
·
材料科学
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Drug Research
·
2023
·Vol. 73
·期 06
·335-340
·
IF 2.2
Guo Haihua,Zhang Rui,Deng Liangjun,Li Meng,Li Sha,Zhao Suqing
Background Inhalation preparation involves liquid or solid raw materials for delivering to lungs as aerosol or vapor. The liquid preparation for nebulizer is effective for convenient use and patient compliance and it has been extensively used in the treatment of clinical lung diseases. Clinical staff often mixes the compound ipratropium bromide with beclomethasone propionate and budesonide inhaler but reference values of inhalants for clinical use need to be established for simplifying the operation procedure. The high-performance liquid chromatography (HPLC) method of compound ipratropium bromide solution, beclomethasone propionate suspension and budesonide suspension after mixed atomization was studied. Methods The specificity, linearity, recovery (accuracy), precision and stability of compound ipratropium bromide, beclomethasone propionate and budesonide were tested to verify the developed liquid phase method. Results The developed liquid phase method had high specificity, linear R2≥0,999, recovery (accuracy) RSD (relative standard deviation) less than 2%, precision RSD less than 2,0%, and stability RSD less than 2,0%. Conclusion The liquid phase methodology developed in this study can be used for the determination of compound ipratropium bromide mixed with beclomethasone propionate and budesonide. The current methodology can also be used to provide a reference for the determination of its content after mixing, and further data support for its clinical medication.
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FOOD CHEMISTRY
·
2020
·
IF 6.306
Qiuhua Wu,Yuhong Song,Qianqian Wang,Weihua Liu,Lin Hao,Zhi Wang,Chun Wang
A magnetic o -hydroxyazobenzene (M-HAzo) porous organic polymer was facilely prepared by a green azo coupling reaction in aqueous solution. The prepared M-HAzo was applied as a new adsorbent for the first time to pre-concentrate phthalate esters (PAEs) from plastic bottled juice, followed by their determination with high performance liquid chromatography-ultraviolet detection. The effects of various parameters, i.e., the mass ratio of the Fe 3 O 4 @SiO 2 to HAzo, extraction time, ionic strength, pH of the sample, desorption conditions were optimized. Under the optimized conditions, the M-HAzo based method exhibited good performance in terms of linear range (0.3–50.0 μg L −1 ), detection limit (0.08–0.50 μg L −1 ), accuracy (recovery of 78.0–115.0%) and repeatability (relative standard deviation of 2.9–7.8%). This work provides a sensitive method for analysis of PAEs at trace levels in drinks, which is featured with high sensitivity, simple operation and environmentally-friendly merit and will have a promising potential in analysis of other organic pollutants.
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Separation Science Plus
·
2018
·Vol. 1
·期 5
·367-373
·
IF 0
Xuemei Wang,Huan Wang,Pengfei Huang,Xiaomin Ma,Xinzhen Du,Xiaoquan Lu
A specific, precise and accurate high-performance liquid chromatography method with ultraviolet detection was established for the simultaneous determination of eight insecticides in fruit samples. Samples were extracted with acetone and cleaned using the quick, easy, cheap, effective, rugged, and safe technique. Under the optimized conditions, wide linearity ranges (5.0–2000 μg kg −1 ) were obtained for the eight insecticides and the correlation coefficients ( r ) ranged from 0.9985 to 0.9994. The limit of detection and limit of quantification were 0.27–1.85 and 0.90–6.18 μg kg −1 , respectively, and acceptable reproducibility (RSD < 6.6% for intra-day, < 9.2% for inter-day) were achieved. The recovery rates for all insecticides at two spiked levels of 20 and 50 μg kg −1 in fruits samples ranged from 85.9 to 110.4%, and the relative standard deviations were in the range of 3.3–8.9%. The results demonstrated clearly that the approach developed provides reliable, simple, rapid and environmentally friendly quantification and identification of eight insecticides in fruits. These results not only gave insights about the insecticides but also contributed to environmental protection and food safety.
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Analytical Methods
·
2018
·Vol. 10
·期 15
·1733-1739
·
IF 2.073
Weixia Li,Ning Chen,Yonggang Zhao,Weiqiang Guo,Nadeem Muhammd,Yan Zhu,Zhongping Huang
N-Nitrosamines (NAs) are potent carcinogens and have been found in food products. Herein we report a simple tandem liquid-phase extraction (TLPE) method coupled with high-performance liquid chromatography (HPLC) for the determination of trace N-nitrosamines (NAs) in food products. The TLPE method is based upon the tandem implementation of pressurized hot water extraction (PHWE) and dispersive liquid–liquid microextraction (DLLME). The target analytes were first extracted with pressurized hot water, and then concentrated into an organic phase (n-octanol) in the DLLME procedure. The TLPE-HPLC system allowed the analytes to be extracted, concentrated and analyzed in a single step with minimal manipulation of the sample preparation, with an overall analysis time of 25 min. The optimized method showed good linearity (r2 ≥ 0.981) and satisfactory recoveries (74–117%) with good repeatability of the extractions (RSDs below 12.8%, n = 5). The limits of detection (LODs) for all nitrosamines in salted duck eggs were in the range of 0.08–0.55 μg kg−1.
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TALANTA
·
2025
·
IF 6.1
Manyan Qiu,Aiai Nie,Jinghang Zhang,Miao Zheng,Ning Guan,Sharuna De,Xiaoyan Pei,Xinyan Yang,Yujun Jiang,Qianyu Zhao,Chaoxin Man
The effective separation of fat-soluble vitamins from complex matrices prior to instrumental analysis remains a significant challenge. Herein, a novel magnetic covalent organic framework (Fe 3 O 4 @tetrakis(4-aminophenyl)methane (TAM)-2,6-dihydroxynaphthalene-1,5-dicarbaldehyde (DHNDA), Fe 3 O 4 @TAM-DHNDA) was successfully designed and prepared for the efficient separation and enrichment of three fat-soluble vitamins in dairy products. The maximal adsorption efficiency of Fe 3 O 4 @TAM-DHNDA to fat-soluble vitamin was as high as 26.94 mg/g. Moreover, the adsorption mechanism of Fe 3 O 4 @TAM-DHNDA for V A , V D , and V E was revealed by molecular simulation techniques. Van der Waals forces and hydrogen bonds were the main interactions between Fe 3 O 4 @TAM-DHNDA and fat-soluble vitamins. Importantly, the magnetic solid phase extraction (MSPE) method based on Fe 3 O 4 @TAM-DHNDA could be used as an effective sample pretreatment technology for separation and enrichment of fat-soluble vitamins from complex matrices prior to instrumental analysis. When coupled with high-performance liquid chromatography-ultraviolet detector (HPLC-UV), the proposed method enables the efficient detection of fat-soluble vitamins in dairy products. The limit of detection (S/N = 3) and limit of quantification (S/N = 10) were achieved at 20–50 ng/mL and 55–150 ng/mL, respectively. Good linearity (R 2 > 0.9998) was obtained within the range of 2–100 μg/mL. The average recoveries of spiked milk samples were determined to be 83%–101% and the relative standard deviation (RSD) was 0.83% to 3.46% ( n =3). This work provides novel insights into the development of novel magnetic adsorbents and the separation and enrichment of fat-soluble vitamins in complex matrices.
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