JOURNAL OF PHARMACEUTICAL SCIENCES
·
2021
·
IF 3.534
Jia Lun,Wenying Zhang,Yu Zhao,Yongbo Song,Xingjie Guo
Dioxopromethazine (DPZ) is a popular phenothiazine antihistamine that is widely used as a racemic drug in clinical to cure respiratory illness. In our work, a reliable, specific, and rapid enantioselective HPLC-MS/MS method has been established and fully validated for the quantification of R- and S-DPZ in rat plasma. After plasma alkalization (with 1 M Na 2 CO 3 ), DPZ enantiomers and diphenhydramine (IS) were extracted using ethyl acetate. Completely separation of R- and S-DPZ (Rs = 2.8) within 12 min was implemented on Chiralpak AGP column (100 × 4.0 mm i.d., 5 μm) employing ammonium acetate (10 mM; pH 4.5) - methanol (90:10, v / v ) as mobile phase. Themultiple reaction monitoring (MRM) mode was used for the detection of DPZ enantiomers and IS. The transitions of m/z 317.2 → 86.1 and 256.2 → 167.1 werechosen for monitoring DPZ enantiomers and IS, respectively. Good linearity (r 2 > 0.995) was achieved for each DPZ enantiomer over the linear ranges of 1.00 - 80.00 ng/mL, with the lower limit of quantitation (LLOQ) of 1.00 ng/mL. The intra-day and inter-day precisions (RSDs,%) were below 12.3%, and accuracies (REs,%) were in the scope of-10.5% to 6.6%, which were within the admissible criteria. The validated bioanalytical approach was applied to the stereoselective pharmacokinetic (PK) research of DPZ in rat plasma for the first time. It was found that significant differences ( p < 0.05) exist between the main PK parameters of R- and S-DPZ, indicating the pharmacokinetic behaviors of DPZ enantiomers in rats were stereoselective. The chiral inversion of the enantiomers did not occur during the assay.
研究领域:
药物分析
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药代动力学
·
生物分析
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DOI
高影响因子
International Journal of Peptide Research and Therapeutics
·
2020
·Vol. 26
·期 4
·2457-2464
·
IF 1.5
Yang Shi-Zhong,Quan Hong-Zhi,Liu Jin-Feng,Gang Hong-Ze,Mu Bo-Zhong
Lipopeptides have potential applications in many industries. It is challenging to quantitatively determine low concentration of lipopeptide. In this paper a highly sensitive and quantitative method for determination of lipopeptide concentration is described. Fatty acids and surfactin were labelled with naphthalene ethylenediamine (NEDA). LC–MS and HPLC with fluorescence detection analyses shown that the surfactins with 2 free carboxyl groups were wholly labelled by 2 NEDA. Linear relationships were found between molar concentration of fatty acids and peak area of labelled fatty acids. Different fatty acids share the same quantitative regression equation and slope of equation due to the reason that each fatty acid was labelled by 1 NEDA. The relationship between surfactin molar concentration and peak area was obtained based on the concentration of the photoluminescent molecule. This method can detect concentrations as low as 3.1 nmol/L, which is less than the limits of the most sensitive method reported for the surfactins previously. The method can also be used to determine other lipopeptides with carboxyl groups.
研究领域:
分析化学
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药学
·
生物技术
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DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2022
·
IF 5.304
Tong Liao,Jia Jia,Kang Tong,Jiuhong Ouyang,Wei Jiang,Xia-ping Zhu
A novel hyper-crosslinked 2, 8, 14, 20-tetraphenyl calix [4] resorcinol arene polymer (HCP-TCRA) was synthesized by using an external crosslinking of 2, 8, 14, 20-Tetraphenyl calix [4] resorcinol arene (TCRA) as monomers and dimethoxymethane as crosslinker. The HCP-TCRA was explored as a SPME fiber coating material. A variety of physicochemical characterization demonstrated that the material has excellent chemical/thermal stability and strong hydrophobicity. The fiber demonstrated fantastic adsorptive property for three synthetic estrogens (diethylstilbestrol, hexestrol, ethinyloestradiol, abbreviated to SESs). In this work, an efficient HCP-TCRA fiber-based SPME method was developed to analyze SESs by coupling with HPLC-MS detection. Under the optimized SPME conditions, this method was shown a wide range of linearity (2.0–100.0 ng mL −1 for diethylstilbestrol, 1.0–100.0 ng mL −1 for hexestrol, and 30.0–480.0 ng mL −1 for ethinyloestradiol), low limits of detection (LODs, 0.5 ng mL −1 for DES 0.3 ng mL −1 for HEX, 10.0 ng mL −1 for EES) and fine reusability (more than 30 times). Finally, the proposed methods had been applied to the determination of SESs in milk samples with a simple pretreatment. At three different levels, relative recoveries presented between 86.7 and 106.4%. The method put up highly sensitive and budget-friendly in detection SESs, and has capacity in quality control of milk products.
研究领域:
分析化学
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食品安全
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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
·
2023
·
IF 3.4
Wanbing Rao,Lijun Li,Chenxia Zhang,Jinfu Zheng,Xiaomei Fan,Baolei Luan,Jiaxiang Sun,Meiyan Qiu,Shuming Wu,Yanhua Li,Zhongqing Wang
A simple and stability-indicating reverse phase high-performance liquid chromatographic (RP-HPLC) method for the determination of rivaroxaban (RIX) and its related substances was developed. Fifteen impurities of RIX, including three unreported isomers, were identified, synthesized, purified, and confirmed using MS, 1 H NMR, 13 C NMR, and HSQC spectral methods. This new method offered baseline separation for all monitored impurities, and was fast and reliable when compared to the European Pharmacopoeia method. Optimum separation for RIX and its related impurities was achieved on an octyldecyl silica column (YMC Core C18, 4.6 ×100 mm, 2.7 µm) by using a gradient HPLC method in 38 min. The final method was validated with respect to precision, LOD and LOQ, linearity, accuracy, and robustness. This developed method was suitable for routine quality control and drug analysis of RIX active substance.
研究领域:
药学
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分析化学
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产品关联
DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF FOOD PROPERTIES
·
2024
·
IF 3.1
Qi-Ju Shao,Yan Wang,Xi-Jin Yang,Ke Su,Jin-Fen Zheng,Li Yang,En-Die Zhou,Xiao-Yan Yuan,Rong-Xiang Chen
Gnaphalium affine is a plant with various active properties and has been approved for use as a traditional medicine and food ingredient. In this study, liquid chromatography with electrochemical detection was utilized to separate the antioxidant compounds of G. affine, in conjunction with liquid chromatography-triple quadrupole mass spectrometry for identification. The in vitro antioxidant activity of G. affine was evaluated using DPPH and ABTS radical scavenging capacity assays, as well as the ferric reducing antioxidant power assay. The results showed that a total of 25 antioxidant compounds were screened and identified, among which 14 compounds were quantitatively analyzed. G. affine was found to be rich in phenolic substances, with the total phenolic content ranging from 14.62 to 59.30 mg GAE/g DW, which exhibited high antioxidant potential. The antioxidant activities showed a strong positive correlation with the total phenolic content (r > 0.9). The predominant phenolic compounds in G. affine were 5-O-caffeoylquinic acid, 3-O-caffeoylquinic acid, ferulic acid, luteolin-7-O-glucoside, 3,5-O-dicaffeoylquinic acid, 1,5-O-dicaffeoylquinic acid, and luteolin, with 3,5-O-dicaffeoylquinic acid and 1,5-O-dicaffeoylquinic acid exhibiting the highest levels. Statistical analysis indicated that monosubstituted caffeoylquinic acids, disubstituted caffeoylquinic acids, and luteolin derivatives strongly correlated with the antioxidant potential. This study identified and quantified the major chemical constituents responsible for the antioxidant properties of G. affine, demonstrating its potential as a natural source of antioxidants for the use in foods, pharmaceuticals, and health products.
研究领域:
植物化学
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药理学
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分析化学
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产品关联
DOI
高影响因子
ANALYST
·
2019
·Vol. 144
·期 23
·6981-6988
·
IF 4.019
Xiaoyan Liao,Fangli Hu,Zilin Chen
Triterpenoids, as an important family of plant secondary metabolites, have important biological activities associated with health and disease prevention. In this work, we proposed a HPLC-MS method for profiling multiple groups of triterpenoid acids and triterpenoid esters differing only in one position of the hydroxyl or methyl group in O. fragrans fruits. A total of thirty-one compounds were identified, and twenty-seven components were discovered in O. fragrans fruits for the first time. The HPLC-MS profiling method was applied in the analysis of the triterpenoids of O. fragrans flowers, and the time courses of triterpenoids of O. fragrans fruits.
研究领域:
分析化学
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植物化学
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植物代谢组学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2020
·Vol. 58
·期 9
·875-879
·
IF 1.28
Qian Zheng-Ming,Fang Bo-Wen,Chen Hai-Ming,Li Chun-Hong,Huang Qi,Chen Ling,Li Wen-Jia,Li De-qiang
In the present study, an online liquid extraction coupled with high-performance liquid chromatography-2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (HPLC-ABTS) system for rapid screening of antioxidants in tea samples was proposed. As an example, the tea samples were firstly extracted by online HPLC extractor with mobile phase at 70°C, then the hyphenated HPLC-ABTS was used for the chromatographic separation on a Poroshell EC C18 column by 0.3% aqueous formic acid and acetonitrile with a gradient elution at 1.5 mL·min−1, and the UV and antioxidant chromatograms with detection wavelengths at 270 nm and 750 nm were recorded, respectively. The established system integrated the processes of online HPLC sample extraction, HPLC separation and online antioxidants detection, the total analysis time of which was <20 min. The developed method was successfully applied to samples of green tea, oolong tea and black tea. As a result, 11 antioxidants were found in tea samples, including gallocatechin, epigallocatechin, catechin, chlorogenic acid, epicatechin, epigallocatechingallate, epicatechingallate, rutin, 1,4,6-trigalloylglucose, quercetin-3-glycoside and kaempferol-3-glucoside. The combined online liquid microextraction and online HPLC-ABTS method is a rapid and green approach for the quality evaluation of tea.
研究领域:
食品科学
·
分析化学
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DOI
PubMed
高影响因子
MOLECULES
·
2017
·Vol. 22
·期 11
·1927
·
IF 2.861
Yanni Cao,Shengzuo Fang,Zhiqi Yin,Xiangxiang Fu,Xulan Shang,Wanxia Yang,Huimin Yang
Cyclocarya paliurusis an edible and medicinal plant containing various bioactive components with significant health benefits. A combinative method using high-performance liquid chromatography (HPLC) fingerprint and quantitative analysis was developed and successfully applied for characterization and quality evaluation ofC. paliurusleaves collected from 18 geographical locations of China. For the fingerprint analysis, 21 common peaks were observed among the 18 samples, and these peaks were identified by high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC–Q–TOF–MS), while a simultaneous quantification of 16 markers was conducted to interpret the variations of contents of these bioactive compounds among theC. paliurusleaves from different geographical locations. Quantification results showed that the contents of these sixteen investigated compounds varied greatly among the leaves from different locations. The developed new method would be a valuable reference for further study and development of this bioactive plant.Keywords:Cyclocarya paliurus;fingerprint;HPLC–Q–TOF–MS;quantitative analysis;quality evaluation
研究领域:
生药学
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分析化学
·
植物科学
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产品关联
DOI
PubMed
高影响因子
Chinese Journal of Natural Medicines
·
2021
·
IF 3
Zheng-Ming QIAN,Zi WU,Qi HUANG,Chuan-Xi WANG,Guo-Yin TAN,Wen-Jia LI,Wan-Yang SUN,Gen-Pin LV,Hao GAO
An eco-friendly and fast HPLC method was developed for the determination of adenosine, inosine, guanosine and uridine in Cordyceps and related products (fermented mycelia of Hirsutella sinensis and Paecilomyces hepiali ). The sample was ultrasonically extracted using 0.5% phosphoric acid solutions for 2.5 min. Sample separation was performed on a Poroshell SB-Aq column (50 mm × 4.6 mm, 2.7 μm) using eco-friendly mobile phase consisting of formic acid and ammonium formate aqueous solution at a flow rate of 1.0 mL·min −1 . The detection wavelength was 260 nm. The developed HPLC method showed good linearity with correlation coefficients of 1.0000 in the test range. Good precision, repeatability and stability of this method were also observed (RSD ≤ 2.81%). The recovery ranged from 91.84%−105.19% (RSD ≤ 2.59%). Compared with reported methods, the current method did not use harmful organic solvent and took only 10.5 min. It obtained a high eco-score of 91 by the “Analytical Eco-Scale” tool. The developed method is eco-friendly and fast, which is suitable for the quality evaluation of Cordyceps and related products.
研究领域:
药学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 34
·期 9
·e4901
·
IF 1.728
Guangjiao You,Chenghao Li,Yingying Mao,Xiaoliang Ren,Yanan Liu,Meng Wang
Radix Paeoniae Alba (RPA) and its processed products are commonly used in traditional Chinese medicine, but the chaos phenomenon among processed products often occurs. In this study, we used multiple chemometric methods to analyze raw and six different processed products of RPA based on HPLC fingerprinting. Heat map analysis was used to assess the changes in chemical composition. Principal component analysis was used for classification, and the samples were divided into four classes: class 1 (raw, wine-processed, and vinegar-processed products), class 2 (bran-processed and soil-processed products), class 3 (stir-fried products), and class 4 (coke products). Further, the orthogonal partial least squares discriminant analysis model was used to obtain chemical markers among different classes. The antioxidant property of RPA is an important factor responsible for its pharmacological effects, and so the antioxidant activity of RPA was also investigated. We measured 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) and hydroxyl radical scavenging ability, and ferric reducing antioxidant power. The total antioxidant activity follows the order: coke > stir-fried > soil-processed > bran-processed > wine-processed > raw > vinegar-processed products. These results suggest that different processing methods affect the chemical composition and antioxidant power of RPA, and thus, different products of RPA should not be mixed.
研究领域:
中药学
·
分析化学
·
药理学
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产品关联
DOI
PubMed
高影响因子
CHIRALITY
·
2024
·Vol. 36
·期 5
·e23672
·
IF 2.8
Chen Chen,Yangfeng Peng,Yongming Wei,Mengyuan Liu,Yu Wang,Siqi Xiong,Huiyi Li,Quan He
Hydroxychloroquine (HCQ), 2-([4-([7-Chloro-4-quinolyl]amino)pentyl]ethylamino)ethanol, exhibited significant biological activity, while its side effects cannot be overlooked. The RP-HPLC enantio-separation was investigated for cost-effective and convenient optical purity analysis of HCQ. The thermodynamic resolution of Rac-HCQ, driven by enthalpy and entropy, was achieved on the C18 column using Carboxymethyl-β-cyclodextrin (CM-β-CD) as the chiral mobile phase agent (CMPA). The effects of C CM-β-CD , pH, and triethylamine (TEA) V% on the enantio-separation process were explored. Under the optimum conditions at 24°C, the retention times for the two enantiomers were t R 1 = 29.39 min $$ {t}_{R1}=29.39\ \min $$ and t R 2 = 32.42 min $$ {t}_{R2}=32.42\ \min $$ , resulting in R s = 1.87 $$ {R}_s=1.87 $$ . The resolution via diastereomeric salt formation of Rac-HCQ was developed to obtain the active pharmaceutical ingredient of single enantiomer S-HCQ. Di-p-Anisoyl-L-Tartaric Acid (L-DATA) was proved effective as the resolution agent for Rac-HCQ. Surprisingly, it was found that refluxing time was a key fact affecting the resolution efficiency, which meant the kinetic dominate during the process of the resolution. Four factors—solvent volume, refluxing time, filtration temperature, and molar ratio—were optimized using the single-factor method and the response surface method. Two cubic models were established, and the reliability was subsequently verified. Under the optimal conditions, the less soluble salt of 2L-DATA:S-HCQ was obtained with a yield of 96.9% and optical purity of 63.0%. The optical purity of this less soluble salt increases to 99.0% with a yield of 74.2% after three rounds recrystallization.
研究领域:
药物化学
·
分析化学
·
制药工程
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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
·
2014
·
IF 2.694
Qinhui Wang,Lei Shi,Xiuling Tang,Qingwei Wang,Xueliang Dang,Yan Zhang
Kushen–Gancao Decoction (KGD) is a classic traditional Chinese herb combination in treating viral hepatitis and chronic liver diseases. This study aims to investigate the pharmacokinetic (PK) study of matrine (MT), oxymatrine (OMT), glycyrrhizic acid (GL) and glycyrrhetinic acid (GA) following oral administration of KGD in rats. A rapid, sensitive and reliable HPLC–MS/MS method was successfully developed for the simultaneous determination of MT , OMT, GL and GA in rat plasma. A Inertsil C 18 analytical column was used with a gradient mobile phase system of methanol-ammonium acetate (5 mM) with a flow rate of 0.5 mL/min. The analysis was performed on a positive and negative ionization electrospray mass spectrometer via multi reaction monitoring (MRM). Linear calibration curves were obtained for the following concentration range: 10–5000 ng/mL for MT, OMT and GL, 50–15,000 ng/mL for GA in rat plasma ( R 2 > 0.99). The lower limit of quantification (LLOQ) was 5 ng/mL (MT, OMT and GL) and 20 ng/mL (GA). The intra- and inter-day accuracies ranged from −7.91 to 9.10% and precisions (RSD) were within 15%. The analytes were found to be stable under short-term temperature conditions, post-preparative temperature conditions, and after three freeze-thaw cycles conditions. The validated method was successfully applied to a pharmacokinetic study in rats after oral administration of KGD.
研究领域:
中药学
·
药理学
·
分析化学
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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）