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TALANTA · 2022 · IF 6.556

Multi-extraction system with identical supported semi-liquid membrane: Enhanced stability for coextraction of acidic and basic drugs

Qianqian Shang,Huajing Liu,Hang Mei,Chuixiu Huang,Xiantao Shen

Coextraction of different groups of analytes is vital for saving sample volumes and simplifying analytical procedures in bioanalysis . Conventionally, coextraction was achieved by using multi-extraction systems with different supported liquid membranes (SLMs). However, the different membrane solvents tended to diffuse into the aqueous solutions and the other SLM to reach distribution equilibrium during extraction process, causing the system instability. In this work, a stable multi-extraction system (integration of liquid-phase microextraction and electromembrane extraction, LPME/EME) based on the identical supported semi-liquid membrane (SsLM) was developed. Principally, the state of distribution equilibrium of the membrane solvent (polypropylene glycol with molecular weight 4000) in SsLM could be reached at the beginning of extraction, which enhanced the coextraction stability. With this multi-extraction system, acidic and basic analytes were simultaneously extracted from practical biological samples. The extraction recoveries of the six model drugs in undiluted urine samples were over 70%. Followed by LC-MS/MS, the limits of quantification (LOQs) were in the range of 5–10 ng mL −1 . The multi-extraction system using the identical SsLM in this study shows promising potential in construction of other stable multi-extraction systems (e.g., LPME/LPME and EME/EME) in the future, which will greatly benefit the group separation of analytes in complicated biological samples.

研究领域: 分析化学 · 生物分析 · 药学
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Separation Science Plus · 2019 ·Vol. 2 ·期 5 ·178-185 · IF 0

Enantioseparation of basic drugs by capillary electrochromatography using a stationary phase of transfersomes

Zhifeng Huang,Yingxiang Du,Xiaoqi Li,Xiaodong Sun,Zijie Feng,Xiaofei Ma

Transfersomes, a special kind of phospholipid vesicles with higher deformability and flexibility, were applied as coating material to prepare a transfersomes-coated capillary column. A capillary electrochromatography enantioseparation system based on the new transfersomes-coated column with carboxymethyl-β-cyclodextrin added to the running buffer as a chiral selector was established for the first time. Compared with a bare column, three basic drugs achieved baseline separation with better resolution (3.17 for Propranolol, 2.38 for Metoprolol, 2.34 for Esmolol) in this transfersomes-electrochromatography system. Several important parameters including concentration of chiral selector, buffer pH and applied voltage were systematically investigated to provide the optimal separation condition. This study constructed a flexible and efficient enantioseparation electrochromatography system with a small amount of transfersomes, and showed that transfersomes as the stationary phase could efficiently improve chiral separation effect.

研究领域: 分析化学 · 药学 · 色谱学
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ANALYTICA CHIMICA ACTA · 2022 · IF 6.911

A feasibility study on the use of hydrophobic eutectic solvents as pseudo-stationary phases in capillary electrophoresis for chiral separations

Ang Li,Song Xue,Yu Xu,Sihui Ding,Di Wen,Qi Zhang

A critical challenge in using deep eutectic solvents (DESs) in capillary electrophoresis (CE) is to develop separation systems in which a DES can really work as a single entity. To achieve this, the authors recently demonstrated a novel strategy that takes advantage of the aqueous dispersibility of hydrophobic DESs (or more accurately hydrophobic eutectic solvents (HESs)). However, the previous work was limited only to the separation of achiral analytes, e.g., analogues, homologues, and isomers. The present study was designed as a follow-up study in order to explore the feasibility of employing HES-type pseudo-stationary phases (PSPs) in CE for chiral separations . By using carboxymethyl-β-cyclodextrin (CM-β-CD) as a model chiral selector, we provide the first evidence that there is a potential synergistic effect between HESs and traditional chiral selectors. Specifically, the combined use of HES (−)-menthol:octanoic acid and CM-β-CD allowed excellent enantioseparations of several basic drugs which were not able to be resolved in the single CM-β-CD system. The enantioresolutions were significantly improved while the migration times of the enantiomers were also shortened due to the hydrophobic mechanism of the HES-type PSP. Critical factors influencing the novel chiral CE system were systematically investigated. Since HESs are considered as “designer” solvents with highly tunable properties, this study demonstrates the potential of employing HESs (or HDES)-type PSPs in CE for chiral separations .

研究领域: 分析化学 · 色谱学 · 分离科学
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MICROCHIMICA ACTA · 2019 ·Vol. 186 ·期 7 ·1-8 · IF 5.479

Metal organic framework HKUST-1 modified with carboxymethyl-β-cyclodextrin for use in improved open tubular capillary electrochromatographic enantioseparation of five basic drugs

Sun Xiaodong,Tao Yu,Du Yingxiang,Ding Wen,Chen Cheng,Ma Xiaofei

This work shows that the metal organic framework (MOF) HKUST-1 of type Cu 3 (BTC) 2 (also referred to as MOF-199; a face-centered-cubic MOF containing nanochannels) is a most viable coating for use in enantioseparation in capillary electrochromatography (CEC). A HKUST-1 modified capillary was prepared and characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectra, elemental analysis and thermogravimetric analysis. CEC-based enantioseparation of the basic drugs propranolol (PRO), esmolol (ESM), metoprolol (MET), amlodipine (AML) and sotalol (SOT) was performed by using carboxymethyl-β-cyclodextrin as the chiral selector. Compared with a fused-silica capillary, the resolutions are improved (ESM: 1.79; MET: 1.80; PRO: 4.35; SOT: 1.91; AML: 2.65). The concentration of chiral selector, buffer pH value, applied voltage and buffer concentration were optimized, and the reproducibilities of the migration times and R s values were evaluated. Schematic presentation of the preparation of a HKUST-1@capillary for enantioseparation of racemic drugs. Cu(NO 3 ) 2 and 1,3,5-benzenetricarboxylic acid (BTC) were utilized to prepare the HKUST-1@capillary. Then the capillary was applied to construct capillary electrochromatography system with carboxymethyl-β-cyclodextrin (CM-β-CD) for separation of basic racemic drugs.

CAS / MDL: 111-30-8 919-30-2
研究领域: 分析化学 · 药学 · 材料科学
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INTERNATIONAL JOURNAL OF PHARMACEUTICS · 2021 · IF 5.875

Sustainable and efficient skin absorption behaviour of transdermal drug: The effect of the release kinetics of permeation enhancer

Jiuheng Ruan,Chao Liu,Haoyuan Song,Ting Zhong,Peng Quan,Liang Fang

At present, how the release kinetics of permeation enhancers affected their enhancement efficacy on drug skin absorption and its molecular mechanisms remained unclear. Herein, the release kinetics of permeation enhancer (Plurol Oleique CC (POCC)) which involved release percent ( PR ), release duration ( RD ) and release kinetic constant ( k ) and its enhancement efficacy on drug skin absorption were investigated with in vitro skin retention study and in vitro skin permeation study, respectively. POCC released from the acidic-drug loading patches followed with the Higuchi release model and had short RD (8–16 h), resulting in its unsustainable enhancement efficiency for acidic drugs. However, POCC released from the basic-drug loading patches followed with zero-order model with long RD (12–24 h), inducing a sustainable and efficient enhancement efficiency for basic drugs. The lower variance of an innovative parameter permeation enhancement coefficient ( C PE ) represented the relatively sustainable and effective enhancement effect and was listed as followed: 0.20 (Zaltoprofen (ZPF)), 0.31 (Diclofenac (DCF)), 0.27 (Indomethacin (IMC)), 0.07 (Azasetron (AST)), 0.11 (Oxybutynin (OBN)) and 0.06 (Donepezil (DNP)). According to the results of FT-IR, MTDSC , 13 C NMR spectra, molecular dynamics simulation, SAXS and Raman imaging, the Higuchi release model was caused by strong interaction between the acid drugs and pressure sensitive adhesive (PSA). This strong interaction induced faster diffusion speed of POCC from acidic-drug loading patches and make the swell degree of long periodicity phase (LPP) of stratum corneum (SC) lipids reached plateau early. The zero-order release model was because the weak interaction between basic drugs and PSA making most of POCC was still bound to PSA, which in turn lead to LPP swelled at a slow but sustainable process. In conclusion, zero-order release kinetic of POCC lead to sustainable and efficient penetration enhancement efficiency on basic drug, while the Higuchi release kinetic showed opposite effect for acidic drugs. A deep understanding of release kinetics of enhancer and its enhancement efficiency may drive the ideal selection of permeation enhancers and rational optimization of transdermal patches .

CAS / MDL: 64-19-7 7664-38-2
研究领域: 药剂学 · 药物递送系统 · 药物化学 · 生物物理学
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