JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
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2018
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IF 0.827
Liwei Cao,Tian Wei,Yihui Shi,Xiaofang Tan,Jianxin Meng
Two rapid and sensitive analytical methods are developed for the determination of D-penicillamine (D-PEN) and tiopronin (TP) through high-performance liquid chromatography with fluorescence detection (HPLC-FLD) and capillary electrophoresis with laser-induced fluorescence detection (CE-LIF). A boron-dipyrrolemethene (BODIPY) fluorescence labeling reagent, 1,3,5,7-tetramethyl-8-bromomethyl-difluoroboradiaza-s-indacene (TMMB-Br) was successfully applied to derivatize these two thiol drugs. Fluorescein was used as the internal standard (IS) for the quantification of D-PEN and TP in CE-LIF. The derivatization and separation conditions were optimized carefully. Under the optimum conditions, the HPLC and CE separation of D-PEN and TP could be achieved within 12 min. The limits of detection were as low as 2.0 nmol/L for HPLC-FLD and 0.47 nmol/L for CE-LIF. The drugs in human urine and serum samples were determined successfully, and the recoveries were 95.0–06.7% and 95.2–104.3%, respectively.
研究领域:
分析化学
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药物分析
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生物医学
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DOI
高影响因子
ANALYTICAL LETTERS
·
2019
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IF 1.248
Bocheng Yu,Zhen Li,Jinyi Wu,Jiamin Ying,Yuqing Tang,Bingchu Wu,Chunlan Tang,Jinyan Xu
A high-performance liquid chromatography with fluorescence detection (HPLC–FLD) and principal component analysis (PCA) and hierarchical cluster analysis (HCA) were developed for the quality control of Gastrodia elata. The developed protocols were successfully applied to the analysis and evaluation of 47 batches of this material from eight regions. A standard fluorescence fingerprint for G. elata was established based on 12 common peaks measured in all samples and the similarities between sample fingerprints and standard fingerprint were almost greater than 0.85. The results of PCA and HCA analysis showed that the samples from the eight regions could be classified into three groups. The correlation between the fingerprints and antioxidant activities was investigated by a stepwise regression model and Pearson correlation analysis. Gastrodigenin and parishin E were screened and validated as potential antioxidant markers of G. elata. This study provides a valuable reference for the evaluation of G. elata and other herbal medicines or their related foods.
研究领域:
中药学
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分析化学
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产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
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2026
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IF 5.2
Xingyu Lu,Youyi Wu,Jingyi Wu,Yuanjie Wang,Shiqian Gao,Xiaofang Shen,Xuedong Wang
A ternary supramolecular deep eutectic solvent (SUPRATDES) consisting of hydroxypropyl-β-cyclodextrin (HP-β-CD), thymol and formic acid was newly synthesized in this work. Based on in-situ derivatization (ISD) and the SUPRATDES, a new vortex-assisted dispersive liquid-liquid microextraction (ISD-SUPRATDES-VA-DLLME) method was first developed and coupled to HPLC-fluorescence detection for the sensitive quantitation of sulfonamides (SAs) residues in water. Upon in-situ derivatizing SAs in sample with fluorescamine and employing the as-synthesized SUPRATDES as the extractant in VA-DLLME procedure, an improvement in comprehensive extraction efficiencies up to 26% was achieved compared with the corresponding DES without β-CD. The important parameters in ISD-SUPRATDES-VA-DLLME were evaluated by one-factor-at-a-time (OFAT) experiments and further optimized by central composite design (CCD). Based on the optimized parameter conditions, the method exhibited an excellent linear range from 0.012 to 300 μg L −1 ( R 2 > 0.9994) and low limits of detection (LOD) ranged from 0.0035 to 0.0076 μg L −1 . Both the intra-day and inter-day precision ( n = 6) were ≤9%, and the obtained enrichment factors (EFs) were varied between 210 and 530. Spiked recoveries of 80.2–114.8% were achieved and insignificant matrix effect (ME of 0.90–1.05) was found for real samples with different matrices. The mechanism of ISD and synergistic extraction of β-CD was investigated with the aid of HPLC-MS, density functional theory (DFT) calculation and molecular docking analysis. This proposed method demonstrated low LODs, high EFs, short extraction time and eco-friendliness, thus offering a novel alternative for the enrichment and detection of multiple SAs in aqueous environment samples.
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DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2024
·Vol. 47
·期 1
·2300545
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IF 2.8
Chen Yang,Jing-Wen Zhang,Jin Qi,Bo-Yang Yu
Pseudoallergy is a typical and common adverse drug reaction to injections, especially in traditional Chinese medicine injections (TCMIs). At present, the evaluation methods for pseudoallergy include cell methods in vitro and animal methods in vivo. The mast cell evaluation method based on the β-hexosaminidase (β-Hex)-catalyzed substrate, 4-nitrophenyl-β-N-acetyl-D-glucosaminide (4-NPG), is an important method for the evaluation of drug-induced pseudoallergy, but it is prone to false positive results and has insufficient sensitivity. In this study, a novel β-Hex evaluation system with rat basophilic leukemia-2H3 cells based on high-performance liquid chromatography-fluorescence detection (HPLC-FLD) was established, which effectively increased the sensitivity and avoided false positive results. Cell viabilities were measured by 3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl tetrazolium bromide assay. In addition, a method for the determination of histamine, which is another indicator in the development of pseudoallergy, was established to validate the above method. The results of this novel method indicated that two TCMIs (Shuxuening injection and Shenqi Fuzheng injection), which were considered to be pseudoallergenic using 4-NPG, were not pseudoallergenic. Overall, the novel β-Hex/HPLC-FLD evaluation system using Rat basophilic leukemia-2H3 cells established was effective and precise. It could be used for the evaluation of pseudoallergic reactions caused by TCMIs and other injections.
研究领域:
药理学
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免疫学
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分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2026
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IF 2.5
Yuxing Liu,Yan Yan,Changjian Wu,Kangwei Shen,Wei Fan,Mengjie Li,Hai Zhao,Yi Cao,Xuejun Kang,Penglin Wu,Dianzhi Liu
PAN/PPy NFs are first applied to PFSPE-HPLC-FLD for urinary pteridines detection. • PAN/PPy NFs adsorb pteridines via synergistic electrostatic, H-bond and π-π forces. • The optimized method gives negligible matrix effects (−6.6%–8.2%) for urine samples. • The sensitive, robust method was fully validated for clinical urine sample analysis. Pteridines are associated with neuroinflammation and oxidative stress, the core pathological processes of autism spectrum disorder (ASD). Urinary neopterin (NPT), biopterin (BPT), and isoxanthopterin (IXP) are promising non-invasive biomarkers for children with ASD. However, matrix interference from urinary salts and metabolites severely impedes trace pteridine detection, while mainstream analytical methods either require cumbersome derivatization or sacrifice sensitivity for dilution to mitigate matrix effects (ME). This study reports the first application of polyacrylonitrile/polypyrrole nanofibers (PAN/PPy NFs) for the determination of pteridines in urine by packed-fiber solid-phase extraction (PFSPE) coupled with HPLC-FLD, without derivatization. XPS, FTIR and fluorescence experiments confirmed pteridine adsorption on PAN/PPy NFs via synergistic electrostatic attraction, hydrogen bonding and π-π stacking. Validation showed: ME -6.6%–8.2%, R 2 > 0.995, LOD s 0.8–5.3 ng/mL, LOQ s 2.8–17.6 ng/mL, and RSD s < 9.7%. AGREE (0.61) and BAGI (72.5) verified its compliance with green analytical chemistry principles. Analysis of 33 ASD and 34 healthy urine samples revealed significantly elevated NPT levels in the ASD group ( p = 0.011). This efficient, sensitive and green PFSPE-HPLC-FLD method eliminates urinary matrix interference without derivatization, overcoming key limitations of conventional approaches. It provides a reliable tool for urinary pteridine assays in ASD research and supports ASD pathogenesis investigation and exploratory clinical studies. The figure shows PAN/PPy-PFSPE for matrix effect elimination from ASD children's urine. PAN/PPy NFs sorbent, with high porosity and multiple interaction sites, mediates pteridine adsorption via synergistic electrostatic attraction, hydrogen bonding and π-π stacking, enabling rapid green purification and ultrasensitive simultaneous detection of urinary NPT, IXP and BPT for exploratory clinical studies. Download: Download high-res image (154KB) Download: Download full-size image
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DOI
PubMed
高影响因子
ANALYTICAL LETTERS
·
2025
·
IF 1.8
Yi Zhang,Jiali Lu,Jiaxiong Zhao,Genrong Li,Shuai Li
This study presents an efficient and highly sensitive method for detecting Rhodamine B and 6 G in complex food matrices. A dual microextraction approach combining electromembrane extraction (EME) and magnetic solid-phase extraction (MSPE) was applied, followed by analysis using high-performance liquid chromatography with fluorescence detection (HPLC-FLD). Critical parameters—such as donor and acceptor phase pH, applied voltage, membrane solvent, extraction time, sorbent dosage, adsorption duration, and elution conditions—were systematically optimized to ensure reliable and reproducible performance. The method showed excellent linearity (1.0–200 ng/mL; R2 = 0.9987 for Rhodamine B and 0.9983 for Rhodamine 6 G), with detection limits of 0.9 ng/mL and 1.2 ng/mL, respectively. Recoveries ranged from 92.1% to 101.9% with relative standard deviations (RSDs) below 5%. Application to real food samples—including spicy strips, candies, and chili oil-based bean snacks—confirmed the method’s accuracy and strong matrix tolerance. Compared to conventional microextraction-chromatographic techniques, this method offers notable advantages in speed, sensitivity, and broad applicability. It is a powerful tool for rapid screening and regulatory monitoring of illicit synthetic dyes in food.
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DOI
高影响因子
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