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RSC Advances · 2023 ·Vol. 13 ·期 12 ·7848-7856 · IF 3.9

In-vial solid-phase extraction of polycyclic aromatic hydrocarbons in drug formulations stored in packaging containing rubber

Hao Yang,Yinmeng Ding,Ya Ding,Jing Liu

Polycyclic aromatic hydrocarbons (PAHs) are a class of ubiquitous and persistent organic compounds that are significantly teratogenic, carcinogenic and mutagenic. Rubber stoppers commonly used in sterile formulation packaging materials often contain carbon black as the additive to enhance mechanical strength. However, PAHs may be formed during the production of carbon black, which could cause the drug formulations to be contaminated when contacting with the rubber stopper, and then enter the patient's body. The determination of PAHs in drug formulations is challenging, due to their trace amounts and matrix interference. Therefore, sample pretreatment is necessary and important. In this work, a novel technique, named in-vial solid-phase extraction (IVSPE), was developed for the selective extraction and enrichment of 16 PAHs in pharmaceuticals. The coated sample vial was directly used as the container for the whole process of sample pretreatment. As the solid-phase adsorbent, the coating was prepared by successively modifying the inner surface of a sample vial with polydopamine film and octadecylamine. PAHs could be selectively extracted through π–π stacking interaction and hydrophobic interaction, and then desorbed and enriched by a small amount of organic solvent. After systematic optimization of the coating preparation and the extraction process, the limits of detection and quantification of 16 PAHs were in the range of 0.002–0.60 ng mL−1 and 0.007–2.00 ng mL−1, respectively. Good linearities and precision of six repeated injections were obtained. The recoveries at three spiked concentration levels in normal saline were in the range of 62.72–106.90% with the relative standard deviation between 0.83% and 6.78%. Finally, PAHs in normal saline and powders for injection were extracted by established IVSPE, followed by separation and detection with high-performance liquid chromatography with a fluorescence detector and diode array detector (HPLC-FLD/DAD). It is worth noting that the preparation conditions of the adsorbent in the IVSPE method are mild, simple and green. Moreover, IVSPE has the advantages of having few work steps and avoiding the risk of contamination, because no special instrumentation or sample transfer is required. IVSPE could also be used for the pretreatment of multiple samples at the same time, which is beneficial to practical applications.

CAS / MDL: 62-31-7 124-30-1
研究领域: 分析化学 · 药学
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ANALYTICAL LETTERS · 2024 · IF 1.6

A Dual-Mode Optical Sensing Strategy for Rapid Detection of D-Penicillamine in Pharmaceutical Formulations

Jin-Wen Liu,Tingting Chen,Meiqun Cai,Yingfeng Qin,Mei Li

Accurate, rapid, and quantitative detection of D-penicillamine (D-PA) in pharmaceutical formulations is imperative for drug quality and clinical medication guidance. Various colorimetric and fluorescent assays have been constructed for D-PA based on nanomaterials. However, the reliable and rapid detection of D-PA in pharmaceutical formulations remains a challenge because these methods suffer from shortcomings such as time-consuming procedures, poor uniformity, and complicated nanomaterial preparation. In this work, an effective and facile homogeneous dual-mode optical sensing strategy was established based on the strong complexation between D-PA and Cu2+ and catalyzed the oxidation of O-phenylenediamine. This platform displayed a sensitive response to D-PA from 5 to 100 µmol/L, with a detection limits of 0.54 µmol/L (fluorescence) and 0.76 µmol/L (colorimetry). As expected, the method was successfully applied to the determination of D-PA in pharmaceutical formulations with satisfactory results. Overall, this developed strategy provides a facile and rapid dual-mode optical platform for D-PA and has great potential in D-PA-related pharmaceutical quality control.

研究领域: 分析化学 · 药学
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LUMINESCENCE · 2015 ·Vol. 31 ·期 1 ·241-246 · IF 1.518

Sensitive determination of enoxacin in pharmaceutical formulations by its quench effect on the fluorescence of glutathione-capped CdTe quantum dots

Qiong Yang,Xuanping Tan,Jidong Yang

A sensitive and simple method for the determination of enoxacin (ENX) was developed based on the fluorescence quenching effect of ENX for glutathione (GSH)-capped CdTe quantum dots (QDs). Under optimum conditions, a good linear relationship was obtained from 4.333 × 10 −9 mol⋅L −1 to 1.4 × 10 −5 mol⋅L −1 with a correlation coefficient (R) of 0.9987, and the detection limit (3σ/K) was 1.313 × 10 −9 mol⋅L −1 . The corresponding mechanism has been proposed on the basis of electron transfer supported by ultraviolet–visible (UV) light absorption, fluorescence spectroscopy, and the measurement of fluorescence lifetime. The method has been applied to the determination of ENX in pharmaceutical formulations (enoxacin gluconate injections and commercial tablets) with satisfactory results. The proposed method manifested several advantages such as high sensitivity, short analysis time, low cost and ease of operation. Copyright © 2015 John Wiley & Sons, Ltd.

CAS / MDL: 70-18-8 74011-58-8
研究领域: 分析化学 · 药学
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JOURNAL OF LUMINESCENCE · 2016 · IF 2.693

Flow-based determination of methionine in pharmaceutical formulations exploiting TGA-capped CdTe quantum dots for enhancing the luminol-KIO4 chemiluminescence

Min Zhou,Ailian Wang,Cong Li,Xiaowei Luo,Yongjun Ma

A novel flow-injection chemiluminescence method (FI-CL) was established for the determination of methionine in this paper, based on its strong enhancement on CL intensity of the luminol-KIO 4 system catalyzed by thioglycolic acid-capped CdTe quantum dots in alkaline media. Under the optimized conditions, the relative CL intensity was in proportion to methionine concentration in the range from 1.0×10 − 8 to 1.0×10 −5   g   mL −1 with a detection limit of 6.6×10 −9   g   mL −1 (3σ). The relative standard deviation (RSD) of the CL intensity for 1.0×10 −6   g   mL −1 standard methionine solution was 0.97% (n=11). The proposed method was successfully applied to determine methionine in commercial pharmaceutical formulations with recoveries between 98.0% and 101.9%. The possible CL mechanism was discussed as well.

CAS / MDL: 521-31-3
研究领域: 分析化学 · 药学
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JOURNAL OF SOLID STATE ELECTROCHEMISTRY · 2011 ·Vol. 16 ·期 2 ·731-738 · IF 2.234

Determination aminopyrine in pharmaceutical formulations based on APTS-Fe3O4 nanoparticles modified glassy carbon electrode

Yin Huanshun,Zhou Yunlei,Liu Tao,Tang Tiantian,Ai Shiyun,Zhu Lusheng

In this work, 3-aminopropyltriethoxysilane modified Fe 3 O 4 nanoparticles (ATPS-Fe 3 O 4 ) were used to modify glassy carbon electrode for aminopyrine determination. ATPS-Fe 3 O 4 showed obviously catalytic activity and adsorptivity towards aminopyrine oxidation proven by the increased oxidation peak current and the decreased oxidation peak potential. The best analytical response was obtained by immobilizing 8 μL 3 mg/mL APTS-Fe 3 O 4 dispersion with an accumulation time of 200 s at −0.2 V in 0.1 M phosphate buffer solution (pH 9.0). The oxidation peak current of aminopyrine showed linear relationship with its concentration in the range from 0.5 to 100 and 100 to 1600 μM. The detection limit was 0.1 μM (S/N = 3). The proposed method showed satisfactory repeatability and anti-interference ability. The fabricated electrode was successfully applied to determine aminopyrine in pharmaceutical formulations.

CAS / MDL: 196504-57-1
研究领域: 分析化学 · 药学
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CHROMATOGRAPHIA · 2011 ·Vol. 75 ·期 1 ·71-76 · IF 1.075

Determination of Six Analgesics by CE with an Improved Electromagnetic Induction Detector

Yang Xiujuan,Feng Jun,Chen Zuanguang,Liao Rifang,Li Xinchun

A novel, rapid and validated capillary electrophoretic method with an improved electromagnetic induction detector has been developed for the determination of ibuprofen, acetaminophen, amantadine hydrochloride, aminopyrine, diclofenac sodium and codeine phosphate in three kinds of analgesic pharmaceutical preparations. Fabrication of the electromagnetic inductor was the same as previously described, but a brand new electric circuit was designed for the detector to lower the background noise and improve the detection sensitivity. Important factors which might influence the response of the detector, including the value of the adjustable inductor and resistor, excitation frequency and voltage, were examined. Electrophoretic parameters affecting separation efficiency, such as variety of buffer, buffer pH, buffer concentration and electroosmotic flow modifier, were also deliberately investigated. Under the optimal conditions, highly linear response was obtained for these six compounds over three orders of magnitude with detection limits ranging from 0.1 to 1.0 μg mL −1 (S/N = 3). The average recovery and RSD were within the range of 97.5–101.5 and 1.1–2.3%, respectively. This simple, convenient, effective and stable method held great promise in quality control of pharmaceutical preparations.

研究领域: 分析化学 · 药学
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LUMINESCENCE · 2010 ·Vol. 26 ·期 6 ·397-402 · IF 1.209

Capillary electrophoresis analysis of isoniazid using luminol-periodate potassium chemiluminescence system

Ying Liu,Zhifeng Fu,Lin Wang

A rapid and simple capillary electrophoresis method coupled with chemiluminescent (CL) detection was proposed for analysis of isoniazid (ISO) based on the enhancement effect of ISO to CL emission of luminol-periodate potassium reaction. Under the optimal conditions, ISO can be assayed in the range of 7.0 × 10 −7 to 3.0 × 10 −5 g mL −1 ( R 2 = 0.9990) with a limit of detection of 3.0 × 10 −7 g mL −1 (signal-to-noise ratio of 3). The whole analysis process can be completed within 2.5 min with a theoretical plate number of 6258. The relative standard deviations of the signal intensity and the migration time were 3.1 and 1.4% for a standard sample at 1.0 × 10 −5 g mL −1 ( n = 5), respectively. The presented novel strategy was successfully applied to the determination of ISO in commercial pharmaceutical preparations and spiked human serum samples. Copyright © 2010 John Wiley & Sons, Ltd.

研究领域: 分析化学 · 药物分析
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Polymers · 2021 ·Vol. 13 ·期 19 ·3351 · IF 4.329

Esterification of Alginate with Alkyl Bromides of Different Carbon Chain Lengths via the Bimolecular Nucleophilic Substitution Reaction: Synthesis, Characterization, and Controlled Release Performance

Xiuqiong Chen,Qingmei Zhu,Chang Liu,Dongze Li,Huiqiong Yan,Qiang Lin

To extend the alginate applicability for the sustained release of hydrophobic medicine in drug delivery systems, the alkyl alginate ester derivative (AAD), including hexyl alginate ester derivative (HAD), octyl alginate ester derivative (OAD), decyl alginate ester derivative (DAD), and lauryl alginate ester derivative (LAD), were synthesized using the alkyl bromides with different lengths of carbon chain as the hydrophobic modifiers under homogeneous conditions via the bimolecular nucleophilic substitution (SN2) reaction. Experimental results revealed that the successful grafting of the hydrophobic alkyl groups onto the alginate molecular backbone via the SN2 reaction had weakened and destroyed the intramolecular hydrogen bonds, thus enhancing the molecular flexibility of the alginate, which endowed the AAD with a good amphiphilic property and a critical aggregation concentration (CAC) of 0.48~0.0068 g/L. Therefore, the resultant AAD could form stable spherical self-aggregated micelles with the average hydrodynamic diameter of 285.3~180.5 nm and zeta potential at approximately −44.8~−34.4 mV due to the intra or intermolecular hydrophobic associations. With the increase of the carbon chain length of the hydrophobic side groups, the AAD was more prone to self-aggregation, and therefore was able to achieve the loading and sustained release of hydrophobic ibuprofen. Additionally, the swelling and degradation of AAD microcapsules and the diffusion of the loaded drug jointly controlled the release rate of ibuprofen. Meanwhile, the AAD also displayed low cytotoxicity to the murine macrophage RAW264.7 cells. Thanks to the good amphiphilic property, colloidal interface activity, hydrophobic drug-loading performance, and cytocompatibility, the synthesized AAD exhibited a great potential for the development of hydrophobic pharmaceutical formulations.Keywords:alkyl alginate ester derivative;bimolecular nucleophilic substitution reaction;controlled release performance;cytocompatibility;hydrophobic pharmaceutical formulations

研究领域: 材料科学 · 药学 · 生物医学工程
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JOURNAL OF MOLECULAR STRUCTURE · 2025 · IF 4.7

Enhancing the solubility and dissolution rate of diflunisal through piperazine stoichiometric variants: Reversible transformation and dissolution advantages

Xian-Rui Zhang,Xiao-Han Zhang,Xian-Ying Xie,Jia-Yu Luo,Hui-Jun Chen,Lei Gao

To overcome the limitations of diflunisal (DIF) regarding its solubility and dissolution rate, two different ratios of DIF-piperazine (PIP) salts were synthesized using a salt formation strategy via proton transfer crystallization. The resulting DIF-PIP salts were characterized using various techniques, including crystal structure analysis, powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), and Fourier transform infrared (FT-IR) spectroscopy. The results demonstrated a significant enhancement in solubility for both the DIF-PIP (1:1) and DIF-PIP (2:1) salts when compared to the DIF active pharmaceutical ingredient (API), with increases of 56.5-fold and 3.7-fold, respectively. Notably, the DIF-PIP (1:1) salt exhibited exceptional dissolution performance across various media. Specifically, its dissolution rates in water, pH 6.86 buffer, and pH 9.18 buffer increased by 338.5-fold, 104.8-fold, and 1.5-fold, respectively. This superior dissolution performance suggests potential advantages for pharmaceutical applications, particularly its high dissolution rate in water, which could improve the disintegration and dissolution properties of oral tablets. Additionally, we investigated the polymorphic transformation conditions between DIF-PIP (1:1) and DIF-PIP (2:1) salts in detail, providing both theoretical and experimental insights into controlling the physicochemical stability of pharmaceutical formulations during preparation and storage.

研究领域: 药学 · 晶体工程 · 药物传递 · 固态化学 · 材料科学
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STRUCTURAL CHEMISTRY · 2023 ·Vol. 35 ·期 3 ·967-975 · IF 1.7

Crystal structures and properties of two aromatic carboxylic acid-based medicinal salts of paliperidone

Shen Zheng,Chen Jian,Ge Jilong,Cai Zhuoer,Hua Xiu-Ni,Sun Baiwang

Two pharmaceutical salts of paliperidone, namely, paliperidone benzoate (PLPT·BA) and paliperidone salicylate (PLPT·SA), were successfully synthesized using benzoic acid (BA) and salicylic acid (SA) as starting materials through a solvent evaporation method. Our study rectified the misidentification of PLPT·BA as a co-crystal in previous research by providing single-crystal structure data and further analysis. The salts’ structures were confirmed through ΔpKa calculations, single-crystal x-ray diffraction (SCXRD) analysis, powder x-ray diffraction (PXRD), and infrared (IR) spectroscopy, while their solubility was also evaluated. Moreover, significant enhancements in thermal stability were observed for both PLPT·BA and PLPT·SA, with increases of 39 K and 32 K, respectively, in their decomposition temperatures compared to pure PLPT. Additionally, intramolecular charge-assisted hydrogen bonds (N + –H···O) were found in both salts, which crystallized in the monoclinic system with the \(P\overline{1}\) P-1 (2) space group. Furthermore, solubility and dissolution rate experiments indicated slight improvements in their solubility and dissolution rate compared to PLPT. This pioneering research provides crucial data on the single-crystal structures and thermal properties of PLPT·BA and PLPT·SA, laying a foundation for further investigations into their potential applications in drug formulations and pharmacology and optimizing drug formulations for enhanced clinical efficacy.

研究领域: 药物化学 · 晶体学 · 材料科学 · 药物研发 · 物理化学
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Analytical Methods · 2012 ·Vol. 4 ·期 6 ·1736-1741 · IF 1.547

Electrochemical behavior of antipyrine at a Bi2S3 modified glassy carbon electrode and its determination in pharmaceutical formulations

Xiaomeng Meng,Zhenning Xu,Mo Wang,Huanshun Yin,Shiyun Ai

A simple electrochemical method based on a Bi2S3 modified glassy carbon electrode (GCE) was developed to determine antipyrine using cyclic voltammetry and differential pulse voltammetry. Antipyrine shows a well-defined oxidation peak at the fabricated electrode in phosphate buffer solution and the oxidation peak current is much higher than that at the bare GCE, indicating that Bi2S3 can effectively improve the oxidation of antipyrine. Several effect factors on antipyrine determination were optimized, such as Bi2S3 amount, solution pH, scan rate and accumulation time. Under the optimal conditions, the oxidation peak current of antipyrine was proportional to its concentration in the range of 2.0 to 100 μM and 100 to 800 μM with a correlation coefficient of 0.9974 and 0.9956, respectively. The limit of detection was estimated to be 0.7 μM (S/N = 3). The developed method showed good reproducibility and excellent anti-interference performance. The fabricated electrode was successfully used to determine antipyrine in pharmaceutical formulations with recovery from 96% to 103.5%.

研究领域: 分析化学 · 电化学 · 药物分析 · 药剂学 · 药物代谢
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Nanomaterials · 2020 ·Vol. 10 ·期 8 ·1513 · IF 4.324

A Versatile and Ultrasensitive Electrochemical Sensing Platform for Detection of Chlorpromazine Based on Nitrogen-Doped Carbon Dots/Cuprous Oxide Composite

Venkata Narayana Palakollu,Rajshekhar Karpoormath,Lei Wang,Jiao-Ning Tang,Chen Liu

The excessive intake of chlorpromazine (CPZ) adversely affects human health profoundly, leading to a series of severe diseases such as hepatomegaly and dyskinesia. The rapid and precise detection of CPZ in real samples is of great significance for its effective surveillance. Herein, a versatile and sensitive electrochemical sensor was developed for the detection of antipsychotic drug CPZ based on a Nafion (Nf)-supported nitrogen-doped carbon dots/cuprous oxide (N-CDs/Cu2O) composite. The as-synthesized N-CDs/Cu2O composite was systematically characterized using various physicochemical techniques. The developed composite-based sensor displayed excellent performance towards CPZ determination in a dynamic linear range of 0.001–230 µM with the detection limit of 25 nM. Remarkably, the developed sensor displayed good performance in terms of sensitivity and selectivity. Furthermore, good anti-interference properties toward CPZ determination were attained despite the presence of highly concentrated interfering compounds. Therefore, this composite could be a notable potential modifier to enhance electrocatalytic activity onto the surface of the electrode. Finally, N-CDs/Cu2O/Nf-based sensor was effectively applied for quantification of CPZ in human urine and pharmaceutical formulation samples.Keywords:electrochemical sensor;carbon dots;cuprous oxide;chlorpromazine;antipsychotic drug;pharmaceutical formulations

研究领域: 分析化学 · 电化学 · 药学 · 材料科学
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