ANALYTICAL CHEMISTRY
·
2024
·
IF 6.7
Tianpei Cai,Xinyue Lei,Hai-Bo Shang,Xia Li,Yetong Guo,Li-Xin Wu,Huwei Liu,Donghao Li
Generally, the traditional stationary phase for liquid chromatography is the key part, but with an in situ immutable property, leading to many separation limitations. Based on the former exploration of photosensitive gas chromatography, we successfully prepared a photosensitive monolithic capillary silica column with high light transmission, taking advantage of the reversible cis–trans isomerism of azobenzene. And the cis–trans isomerism has launched an effective, reversible, and precise control on the liquid chromatographic retention behavior just by photoinduction according to the theoretical basis of a good correlation between photoinduction time, trans-azobenzene ratio, and chromatographic retention factor (k) (R2 > 0.9586). In this system, the plausible control mechanism of stationary phase’s polarity is the synergistic effect of the self-molecular polarity difference and the occupation (or release) of polar groups on the stationary phase surface by cis–trans isomerism. Furthermore, a “light control–time ratio cycle” strategy was first reported to maintain an arbitrary ratio of trans-azobenzene corresponding to the polarity gradient of the stationary phase during the whole chromatographic separation process, which is verified by a close correlation of the retention time of the targets and the ratio of light-controlled time (R2 > 0.9977). The “gradient elution” of the targets was also surprisingly realized due to the gradient regulation of stationary phase’s polarity by the programmatic control of alternate light induction and time ratio. This work further advances the practical significance of photosensitive chromatography in “one column for multiple columns”, even “one column for multidimensional chromatography”, and truly provides research foundation for its development in the separation and analysis of complex biological samples.
研究领域:
分析化学
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色谱技术
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DOI
PubMed
高影响因子
SEPARATION AND PURIFICATION TECHNOLOGY
·
2020
·
IF 5.774
Yi Yang,Jing Meng,Haoquan Li,Dongyu Gu,Shuai Wang,Shuai He,Haiyu Xu,Yoichiro Ito
In the present study, high-speed counter-current chromatography with a three-phase solvent system composed of n -hexane-acetonitrile-400 mM ammonium sulfate (1:1:1, v/v) was developed to recover four mixed dyes (methyl green, acridine orange, Congo red and oil red O) with diverse polarities. As a result, four dyes were successfully separated in a single HSCCC run using a step-wise gradient elution. Then, elution-extrusion and back-extrusion counter-current chromatography were used to reduce the separation time and solvent consumption. Among them back-extrusion CCC can save more time. Thus, the present study provides an effective method for dye recycling.
研究领域:
分析化学
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环境科学
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DOI
高影响因子
Analytical Methods
·
2023
·Vol. 15
·期 7
·884-895
·
IF 3.1
Xin Wang,Xiaoqi Sun,Yueying Jin,Shengyu Cheng,Yu Han,Minghui Zhang,Lingli Zhang,Xi-Ling Li,Chun-Yan Xu,Jun Zhe Min
This study reports a novel fluorescent chiral derivatization reagent, 4-(N,N-dmethylaminosulfonyl)-2,1,3-benzoxadiazole-(2-succinimidoxy)-trans-2-methyl-L-proline (DBD-S-M-Pro), with a benzoxadiazole structure containing an N-hydroxysuccinimide activation group. DBD-S-M-Pro targets chiral amino-functional compounds under alkaline conditions without a condensation agent. Gradient elution was performed on a BEH C18 (100 × 2.1 mm, 1.7 μm) column with a mobile phase of 0.05% formic acid (FA) in 10 mM ammonium acetate (CH3COONH4) and 0.1% FA in acetonitrile or methanol. The efficiency of the chiral resolution was evaluated under excitation and emission wavelengths of 450 nm and 560 nm, respectively. The 19 chiral amino acids were separated in the range of 1.45–14.84. The resolutions of almost all DL-amino acids exceeded 1.5; the exceptions were serine (Ser) and lysine (Lys), with resolutions of 1.45 and 1.46, respectively. In addition, a new approach was devised for the simultaneous analysis of four chiral amino acids (DL-Glu, DL-Ala, DL-Val, and DL-Phe) in human hair. These amino acids were analyzed in the range of 12.5–400 pmol, with R2 ≥ 0.9990, limits of detection (S/N = 3) of 4–10 pmol, and intraday and interday precisions of 0.57–6.23%. The average spikes in the hair recoveries were 89.76–111.54%, and the matrix effects were 92.47–102.40%. Next, the contents of free chiral amino acids in the hair samples of 10 healthy volunteers (five males and five females) were analyzed with this method, and the differences were compared. The developed DBD-S-M-Pro provides a novel strategy for the sensitive determination of free chiral amino acids in living organisms.
研究领域:
分析化学
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生物化学
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药学
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DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2024
·Vol. 47
·期 12
·2400247
·
IF 2.8
Xiang-Ling Qin,Si-Yu Wang,Qi-Long Li,Jun-Jie Wang,Zhong-Wei Yao,Jin-Hao Zhu,Lin-Xia Chen,Jie-Ge Huo,Song-Lin Li,Jing Zhou,He Zhu
Glutathione (GSH) is an important antioxidant that is generated and degraded via the GSH cycle. Quantification of the main components in the GSH cycle is necessary to evaluate the process of GSH. In this study, a robust ultra-performance liquid chromatography-tandem mass spectrometry method for the simultaneous quantification of 10 components (GSH; γ-glutamylcysteine; cysteinyl-glycine; n -acetylcysteine; homocysteine; cysteine; cystine; methionine; glutamate; pyroglutamic acid) in GSH cycle was developed. The approach was optimized in terms of derivative, chromatographic, and spectrometric conditions as well as sample preparation. The unstable thiol groups of GSH, γ-glutamylcysteine, cysteinyl-glycine, n -acetylcysteine, cysteine, and homocysteine were derivatized by n-ethylmaleimide. The derivatized and underivatized analytes were separated on an amino column with gradient elution. The method was further validated in terms of selectivity (no interference), linearity (R 2 > 0.99), precision (% relative standard deviation [RSD%] range from 0.57 to 10.33), accuracy (% relative error [RE%] range from -3.42 to 10.92), stability (RSD% < 5.68, RE% range from -2.54 to 4.40), recovery (RSD% range from 1.87 to 7.87) and matrix effect (RSD% < 5.42). The validated method was applied to compare the components in the GSH cycle between normal and oxidative stress cells, which would be helpful in clarifying the effect of oxidative stress on the GSH cycle.
研究领域:
分析化学
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生物化学
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药理学
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细胞生物学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Yang Huang,Ying Feng,Guangyun Tang,Minyi Li,Tingting Zhang,Marianne Fillet,Jacques Crommen,Zhengjin Jiang
Flavonoids from plants always show a wide range of biological activities. In the present study, a rapid and highly efficient supercritical fluid chromatography (SFC) method was developed for the separation of 12 flavonoids. After careful optimization, the 12 flavonoids were baseline separated on a ZORBAX RX-SIL column using gradient elution. A 0.1% phosphoric acid solution in methanol was found to be the most suitable polar mobile phase component for the separation of flavonoids. From the viewpoint of retention and resolution, a backpressure of 200 bar and a temperature of 40 °C were shown to give the best results. Compared with a previously developed reverse phase liquid chromatography method, the SFC method could provide flavonoid separations that were about three times faster, while maintaining good peak shape and comparable peak efficiency. This SFC method was validated and applied to the analysis of five flavonoids (kaempferol, luteolin, quercetin, luteoloside, buddleoside) present in Chrysanthemum morifolium Ramat. from different cultivars (Chuju, Gongju, Hangju, Boju). The results indicated a good repeatability and sensitivity for the quantification of the five analytes with RSDs for overall precision lower than 3%. The limits of detection ranged from 0.73 to 2.34 μg/mL, while the limits of quantification were between 2.19 and 5.86 μg/mL. The method showed that SFC could be employed as a useful tool for the quality assessment of Traditional Chinese medicines (TCMs) containing flavonoids as active components.
研究领域:
分析化学
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生药学
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药物分析
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
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.
研究领域:
分析化学
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药物分析
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色谱学
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手性分离
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药理学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL BIOCHEMISTRY
·
2023
·
IF 2.9
Yao Liu,Zhichao He,Heng Liang,Minzhen Han,Jinxingyi Wang,Qian Liu,Yanping Guan
Rapidly developing UHPLC-MS/MS bioassays with high throughput and quality are challenging yet desired in routine clinics. Methods & results A high-throughput UHPLC-MS/MS bioassay has been built for simultaneously quantifying gefitinib , ruxolitinib , dasatinib , imatinib , ibrutinib , methotrexate , cyclophosphamide and paclitaxel . After the protein precipitation with methanol, samples were separated on an Acquity BEH C 18 column following a gradient elution system with methanol and 2 mM ammonium acetate in water at 40 °C with a run time of 3 min (flow rate 0.4 mL/min). Mass quantification in the positive ion SRM mode was then performed with electrospray ionization . The method of specificity, linearity, accuracy, precision, matrix effects, recovery, stability, dilution integrity and carryover were all validated as per the guideline of the China Food and Drug Administration whose values met the admissible limits. Application of the bioassay to therapeutic drug monitoring revealed important variability in the studied anti-tumour drugs. Conclusion This validated approach was shown to be reliable and effective in clinical management, being a valuable support in therapeutic drug monitoring and subsequent individualized dosing optimization.
研究领域:
药理学
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临床医学
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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 SEPARATION SCIENCE
·
2022
·Vol. 45
·期 13
·2161-2176
·
IF 3.614
Yan-lin Zhao,Lin-lin Zhao,Yu-xin you,Xiao-xiao Zheng,Yan Du,Dao-quan Tang
We aim to establish a simple and easy high-performance liquid chromatography system coupled with an ultraviolet detector suitable for simultaneous determination of 24 antiepileptic drugs in human plasma. Optimized chromatographic separation was performed on a ZORBAX Eclipse Plus-C18 (4.6 × 150 mm 2 , 3.5 μm) column with acetonitrile and 5 mM potassium dihydrogen phosphate water solution as mobile phase. Note that, 24 antiepileptic drugs were divided into three groups and eluted with different gradient procedures, respectively. The column temperature was maintained at 35°C and the detection wavelength was set at 210 nm. Plasma was processed with ethyl acetate or acetonitrile. The calibration curves of 24 antiepileptic drugs demonstrated good linearity within the test range ( r > 0.996). The intra- and inter-batch precision and accuracy were all less than 15%, while extraction recoveries were in the range of 74.57–90.89% with the relative standard deviation values less than 15%. The validated methods have been successfully applied to determination of some antiepileptic drugs in rat or patient plasma. Those results indicated that the developed methods were simple and easy, and could be suitable for the determination of 24 antiepileptic drugs in plasma just by changing the gradient elution procedures of mobile phase.
研究领域:
分析化学
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药理学
·
临床化学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Yufeng Shen,Huiliang Geng,Feifang Zhang,Zongying Li,Bingcheng Yang
A polyethyleneimine (PEI)-functionalized polymer substrate polar stationary phase was prepared for hydrophilic interaction chromatography (HILIC) by grafting PEI onto poly(styrene-divinylbenzene) (PS-DVB) microspheres. The phase shows a U-shape retention profile and it exhibits typical hydrophilic characteristic when the organic solvent fraction in the mobile phase is > 60%. Hydrogen bonding, anion exchange, and hydrophobic interaction are involved in the retention mechanism. Good separation and unique selectivity for acidic, basic and neutral polar analytes were achieved. It showed extremely low column bleed (comparable to that of blank) under gradient elution mode (even to 50% fraction of water) and wide pH tollerance range (at least 1–13).
研究领域:
分析化学
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色谱学
·
材料科学
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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）