SENSORS AND ACTUATORS B-CHEMICAL
·
2017
·
IF 5.401
Lisha Zhang,Pei Song,Hao Long,Meng Meng,Yongmei Yin,Rimo Xi
Amlodipine is one of the most important anti-hypertension agents and S-amlodipine is 1000 folds more efficient than R-amlodipine. However, chiral separation of amlodipine remains a challenge. Here we present an effective strategy for chiral resolution of amlodipine using anti-S-amlodipine antibody for ultra-specific capture and magnetic beads for convenient collecting. The collected enantiomers are ultra-pure based on the chiral HPLC identification. Simultaneously, the captured S-amlodipine could be quantitatively detected with a linear range from 0.1 to 1000 ng mL −1 ( R 2 = 0.9937), along with a limit of detection of 0.04 ng mL −1 . The advantages of the developed magnetic electrochemical biosensor for amlodipine include specific chiral separation, sensitive quantitation, easy-to-operate procedures and time-saving protocols. This method is demonstrated as a novel tool for highly confident separation and quantification of amlodipine enantiomers, in this study. The magnetic biosensor may open up new avenues for intensive study of amlodipine enantiomers and thus be potential in clinical pharmacy and pharmacokinetics studies.
研究领域:
药理学
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分析化学
·
生物医学工程
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产品关联
DOI
高影响因子
ANALYTICAL CHEMISTRY
·
2021
·
IF 6.986
Zhu-Jun Zhong,Zhong-Ping Yao,Zi-Qi Shi,Yang-Dan Liu,Li-Fang Liu,Gui-Zhong Xin
Nitric oxide (NO) is a molecule of physiological importance, and the function of NO depends on its concentration in biological systems, particularly in cells. Concentration-based analysis of intracellular NO can provide insight into its precise role in health and disease. However, current methods for detecting intracellular NO are still inadequate for quantitative analysis. In this study, we report a quantitative mass spectrometry probe approach to measure NO levels in cells. The probe, Amlodipine (AML), comprises a Hantzsch ester group that reacts with NO to form a pyridine, Dehydro Amlodipine (DAM). Quantification of DAM by ultraperformance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) allows specific measurement of intracellular NO levels. Notably, the AML/NO reaction proceeds rapidly (within 1 s), which is favorable for NO detection considering its large diffusivity and short half-life. Meanwhile, studies under simulated physiological conditions revealed that the AML response to NO is proportional and selective. The presented UPLC–MS/MS method showed high sensitivity (LLOQ = 0.24 nM) and low matrix interference (less than 15%) in DAM quantification. Furthermore, the mass spectrometry probe approach was demonstrated by enabling the measurement of endogenous and exogenous NO in cells. Hence, the quantitative UPLC–MS/MS method developed using AML as a probe is expected to be a new method for intracellular NO analysis.
研究领域:
分析化学
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生物化学
·
药理学
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产品关联
DOI
PubMed
高影响因子
CHEMICAL ENGINEERING JOURNAL
·
2019
·
IF 8.355
Shuai Shao,Li Qian,Xin Zhan,Mengjie Wang,Kun Lu,Jianbiao Peng,Dong Miao,Shixiang Gao
Amlodipine (AML), an antihypertensive drug, has raised great environmental concerns due to the widespread occurrence in wastewater for its extensive use. In this study, we introduced an effective approach for AML removal via an oxidation reaction with peroxymonosulfate (PMS) activated by magnetic cobalt ferrite (CoFe 2 O 4 ), and highlighted the governing role of PMS concentration in the degradation process. Nearly complete removal of 10 μM AML (92.5%) was achieved in 30 min with 25 μM PMS and 40 mg/L CoFe 2 O 4 at neutral condition (pH 7.0), while the mineralization was negligible. To enhance the mineralization of AML, PMS concentration was further increased to 10 mM with the mineralization of 70.2%. A total of eight intermediates were identified using liquid chromatography-time-of-flight-mass spectrometry analysis in combination with frontier electron densities calculations, and two major transformation pathways including hydroxylation and dehydrogenation were proposed. Temporal evolution of the intermediates was monitored, of which the differences were tracked as PMS concentration increased from 25 μM to 1.2 mM. Toxicity changes throughout the degradation process were assessed on ECOSAR program, indicating that higher PMS concentration of 1.2 mM led to further reduction of potential threats, although the toxicity of some intermediates with pyridine structure needs to be further validated. Based on the findings in this study, CoFe 2 O 4 /PMS appears to be a promising alternative to remove AML from aquatic environment when appropriate PMS concentration is selected for more pronounced performance.
研究领域:
环境科学
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药理学
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DOI
高影响因子
Analytical Methods
·
2014
·Vol. 6
·期 12
·4408-4413
·
IF 1.938
Jiaqi Xie,Qi Tan,Lin Yang,Shenzhi Lai,Shaotan Tang,Changqun Cai,Xiaoming Chen
A simple, rapid and sensitive method for chiral separation of the amlodipine racemate was developed. (R)- and (S)-amlodipine enantiomers were separated by achiral HPLC, utilising dual chiral mobile phase additives, within 16 min, which was much faster than the previous similar studies. The method was established on an achiral WondaSil C18 column, using methanol–water (45 : 55 (v/v), pH 2.5) containing 7.5 mmol L−1 sulfobutylether-β-cyclodextrin (SBE-β-CD) and 0.3 mmol L−1 polyethylene glycol-20 000 (PEG-20M) as the mobile phase. Effects of additives and concentration, content of methanol and pH on the enantioseparation were investigated. The method was validated for linearity, repeatability, limits of detection (LOD) and limits of quantification (LOQ). The calibration curve (R(S)2 = 0.9998) was constructed in the range of 10–500 μg mL−1 for (S)-amlodipine. Repeatability (n = 6) showed less than 2% relative standard deviation (R.S.D.). LOD and LOQ were found to be 0.032 and 0.106 μg mL−1 for (S)-amlodipine. This method was flexible, simple and economically advantageous over the use of a chiral stationary phase, and was successfully applied to the determination of the amlodipine enantiomers in a commercial pharmaceutical tablets study.
研究领域:
药物分析
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分析化学
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DOI
高影响因子
CHIRALITY
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2020
·Vol. 32
·期 8
·1062-1071
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IF 2.171
Min Liu,Zhong-Qian Liu,Hai Zhu,Chao-Hong He,Ke-Jun Wu
In this paper, a novel l -glutamate based immobilized chiral ionic liquid (SBA-IL (Glu)) was prepared by chemical bonding method and applied as a solid sorbent for chiral separation of amlodipine. The performance of SBA-IL (Glu) was investigated for the absorption of ( S )-amlodipine and separation of amlodipine enantiomer. The static experiment showed that equilibrium adsorption was achieved within 80 minutes, and the saturation adsorptions capacity was 12 mg/g. The complex was then packed in a glass chromatographic column for the separation of amlodipine and the enantiomeric excess (%ee) of ( S )-amlodipine reached 24.67%. The immobilized ionic liquids exhibit good reusability, and the separation efficiency remains 18.24% after reused five times, which allows potential scale-up for the chiral separation of amlodipine.
研究领域:
药物化学
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分析化学
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DOI
PubMed
高影响因子
LUMINESCENCE
·
2020
·Vol. 36
·期 3
·668-673
·
IF 1.855
Xiao Gao,Mingwei Guo,Ming Liu,Li Zhang,Zhiyi Yao
In this report, we develop a dual-output sensor with fluorometric and colorimetric responses, for the rapid and simple detection of berberine hydrochloride (BRH) in 100% aqueous solution based on an anionic polythiophene derivative, poly(2-(2-(4-methylthiophen-3-yloxy)-ethyl) malonic acid) (PTMA). The sensing performance and mechanism were carefully examined by absorption and emission spectra. It can be applied to quantitatively detect BRH in aqueous solution with a detection limit 0.27 μM. The appealing performance of the sensor was demonstrated to originate from the electrostatic and π–π interactions between PTMA and BRH, which promoted the conformational change and aggregation of the PTMA backbone. Moreover, this method allowed rapid detection of BRH in urine samples and BRH tablets with high accuracy.
研究领域:
分析化学
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药物分析
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材料科学
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DOI
PubMed
高影响因子
CHEMOSPHERE
·
2021
·
IF 7.086
Mengjie Wang,Huanhuan Shi,Shuai Shao,Kun Lu,Hanyu Wang,Yun Yang,Zhimin Gong,Yuegang Zuo,Shixiang Gao
The photolysis of amlodipine (AML) as a ubiquitous pollutant in natural water has been extensively studied. Montmorillonite (MMT), a major component of suspended particles in surface aquifers, plays key roles in the natural transportation and transformation of organic contaminants in the environment. However, literature has scarcely focused on whether and how suspended particles affect the phototransformation of AML. This study systematically investigated the phototransformation behavior of AML in MMT suspensions under simulated sunlight. The results obtained showed that MMT significantly enhanced the photolysis of AML. The photodegradation of AML in 0.05 g/L MMT suspension reached 92.2 % after 3 h irradiation under the simulated sunlight. The photodecomposition followed the pseudo-first-order kinetic with a rate constant of 0.803 h −1 in the presence of 0.05 g/L MMT, which is about 19 times larger than that in the absence of MMT (0.0421 h −1 ). Further mechanistic investigation suggested that MMT accelerated the photolysis of AML by the formation of surface complexes between cationic amino groups of AML and the negatively charged sites on MMT surface, which greatly facilitated light absorption and electron transfer for the production of cationic radical AML +· . Meanwhile, the hydroxyl radicals generated by irradiated MMT also played an important role in the photocatalytic degradation of AML. The probable photodegradation pathways of AML in MMT suspension further supported the proposed mechanisms. The toxicity evaluation of phototransformation products of AML with ECOSAR program indicated that photolysis could reduce its potential threats. These findings reveal an important and previously overlooked phototransformation mechanisms of AML in the presence of MMT clays, which is of importance in assessing the environmental fate of other similar organic contaminants.
研究领域:
环境科学
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污染控制
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药学
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DOI
高影响因子
ANALYTICAL CHEMISTRY
·
2025
·
IF 6.7
Xin Qian,Lan Xia,Baian Ji,Yike Huang,Zhining Xia
To improve separation efficiency and address the adverse effects of electro-osmosis, a coated capillary was used to shield the electroosmosis. A nanoflow pump was used to control the flow of the electrophoretic medium, thereby extending the time of the electrophoretic action. Furthermore, by using a coated capillary that is only 10 cm long as the separation column, the electric field strength could reach as high as 250 V/mm. These strategies strengthened the interaction between the enantiomers and the chiral selector, thus enhancing the resolution of enantiomers. As a result, complete separation of the amlodipine enantiomers could be achieved by halting the electrophoretic medium. Further extending the duration of flow stoppage can increase the resolution several-fold. The method established in this study exhibits excellent accuracy and precision. Despite experiencing a long period of flow stoppage, the relative standard deviations of both migration time and resolution remain less than 2%. This method not only remarkably enhanced the resolution of amlodipine enantiomers but also demonstrated broad applicability in separating other chiral enantiomers, particularly for those substances that are difficult to separate using conventional capillary electrophoresis.
研究领域:
分析化学
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药物分析
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生物化学
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产品关联
DOI
PubMed
高影响因子
Water
·
2020
·Vol. 12
·期 11
·3150
·
IF 2.544
Jianye Xu,Siqi Zhou,Erdeng Du,Yongjun Sha,Lu Zheng,Mingguo Peng,Ling Ling
The UV/chlorine process, as a new type of AOP (Advanced Oxidation Process), was utilized to treat amlodipine (AML)-containing water. The influencing factors, including chlorine dose, UV intensity, solution initial pH value, and ammonia concentration, were investigated. The degradation of AML in real water and the relative contributions of OH• and Cl• were also studied. Finally, high-resolution mass spectrometry (HRMS) and GC-MS were used to identify the possible degradation products. The results demonstrated that the AML degradation process was fitted with apparent first-order kinetics. AML degradation had a positive correlation with UV intensity and chlorine dose, and a negative correlation with ammonia concentration. In the presence of ammonia nitrogen and DOM, the removal of AML from real water was reduced. OH• made a dominant percentage contribution of 55.7% to the degradation of AML. Sixteen intermediates were detected and identified. A possible degradation mechanism was also proposed. Acute toxicity tests and risk prediction both illustrated that the complete removal of AML does not guarantee the reduction of acute toxicity, but a prolonged degradation promoted the detoxification of toxic intermediates. The UV/chlorine process can be regarded to be an effective method to remove AML and reduce ecological risk.Keywords:Amlodipine;UV/chlorine;influencing factors;degradation products;ecological risk
研究领域:
环境科学
·
毒理学
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产品关联
DOI
高影响因子
BRAZILIAN JOURNAL OF CHEMICAL ENGINEERING
·
2022
·Vol. 39
·期 3
·661-669
·
IF 1.772
Jin Zhengwei,Yu Changjun,Wang Ruyang,Wei Wei,Jing Yunhuan,Wang Qi
The production of precipitated calcium carbonate (PCC) from carbonate-free minerals and CO 2 from industrial exhaust gas could lower energy consumption and promote CO 2 sequestration. The present study proposes a chemical looping process for the production of PCC from wollastonite (calcium silicate) and CO 2 from industrial exhaust using ammonium chloride as the looping medium; this study also included a pilot setup with a capacity of 3 kg of carbonate per hour to demonstrate the process. The process consisted of three phases: extraction of calcium from the wollastonite with hydrochloric acid; carbonation of the CO 2 in the extract solution in the presence of ammonia to produce calcium carbonate while generating ammonium chloride; and regeneration of hydrochloric acid and ammonia by the decomposition of ammonium chloride. A special air-lift reactor with an integrated settling vessel was designed for the carbonation reaction. The extraction and carbonation conditions were optimized, and fine calcium carbonate with a purity greater than 98% and a particle size of 2 μm was produced. The overall utilization of the calcium from wollastonite and the CO 2 reached 99 and 90%, respectively. This process avoids the high-temperature pyrolysis of limestone and thus consumes less energy. It also sequesters CO 2 from industrial exhaust and is a green and high-performing process for the production of PCC.
研究领域:
化学工程
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环境科学
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产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Shiqi Wang,Jiahui Wu,Qingcheng Wang,Yunfeng Zhang,Hong Yuan,Jianding Wang,Yonghui Wu,Yaxi Xu,Na Ji,Bin Quan,Haixing Wang,Qing Shen
A miniature mass spectrometer (mMS) based point-of-care testing (POCT) method was evaluated for on-site detecting the hypertension drugs, amlodipine and benazepril . The instrument parameters, including voltage, ISO1, ISO2, and CID , were optimized, under which the target compounds could be well detected in MS 2 . When these two drugs were injected simultaneously, the mutual ionization inhibition and mutual reduction between amlodipine and benazepril were evaluated. This phenomenon was severe on the precursor ions but had a small impact on the product ions, thus making this POCT method suitable for analysis using product ions. Finally, the method was validated and applied. The blood samples from patients were tested one hour after oral administration of the drugs (20 mg), and the benazepril was quantitatively analyzed using a standard curve, with detected concentrations ranging from 190.6 to 210 μg L −1 and a relative standard deviation (RSD) of 8.6 %. In summary, amlodipine has low sensitivity and can only be detected at higher concentrations, while benazepril has high sensitivity, good linearity, and even meets semi-quantitative requirements. The research results of this study are of great clinical significance for monitoring blood drug concentrations during hypertension medication, predicting drug efficacy , and customizing individualized medication plans.
研究领域:
分析化学
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临床医学
·
药理学
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产品关联
DOI
PubMed
高影响因子
SEPARATION AND PURIFICATION TECHNOLOGY
·
2020
·
IF 5.774
Lelin Zeng,Qian Liu,Bart Van der Bruggen,Kewen Tang,Xiang Yi,Guoxiang Wang
An integrated separation process is proposed for recovery and enantioseparation of a chiral antihypertensive drug amlodipine from wastewater. Utilizing this integrated technology, both high recovery ( Y ) and high enantiomeric excess ( ee ) were obtained due to the strong enrichment ability of supported liquid membrane with strip dispersion (SLM-SD) and the good enantioseparation ability of organic phase crystallization. These two steps were coupled by an intermediate step: aqueous phase crystallization. In the SLM-SD, an extractant P204 (bi(2-ethylhexyl)phosphoric acid) was dissolved in n -heptane to form a liquid membrane phase, and hydrochloric acid was used as stripping agent. One-stage SLM-SD recycled the amlodipine from wastewater into a stripping phase with a removal ( E AD ) of 99.67% and a Y 1,AD of 87.91% after optimizing the parameters: pH and the concentrations of P204, hydrochloric acid, and amlodipine. Sodium hydroxide and ( L )-tartaric acid were added into the stripping aqueous phase to obtain amlodipine-1/2( L )-tartrate acid crystals, which were directly used in the subsequent organic phase crystallization without tedious additional steps. The Y 2, AD of aqueous phase crystal reached 99% at a pH of over 6.68 and a molar ratio of over 0.5 for ( L )-tartrate acid to amlodipine. Using ( L )-tartaric acid or ( D )-tartaric acid as resolving agent and dimethylsulfoxide as solvent, high-value-added products ( R )-amlodipine and ( S )-amlodipine were obtained by two steps of organic phase crystallization. The ee of products was over 99% after optimizing the dosages of dimethylsulfoxide and resolving agent. To increase the total yield, the generated mother liquors were re-treated by SLM-SD with the recovery of over 99% for residual amlodipine.
研究领域:
环境科学
·
制药工程
·
化学工程
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）