Brazilian Journal of Pharmaceutical Sciences
·
2023
·
IF 1.3
Mei Xuejiao,Lu Dingqiang,Yan Xiangping
L-Malic acid is the Active Pharmaceutical Ingredient of the latest generation of compound electrolyte injection (STEROFUNDIN ISO, Germany) and plays a very important role in the rescue of critically ill patients. The optical purity of L-malic acid is a Critical Quality Attributes. A new reversed-phase high performance liquid chromatography (RP-HPLC) method for pre-column derivatization of D-malic acid enantiomer impurity in L-malic acid bulk drug was established. The derivatization reaction was carried out using (R)-1-(1-naphthyl)ethylamine ((R)-NEA) as a chiral derivatization reagent. The Kromasil C18 column was used with a detection wavelength of 225 nm, a flow rate of 1.0 mL·min-1, and a column temperature of 30 °C. The mobile phase was acetonitrile-0.01 mol·L-1 potassium dihydrogen phosphate solution (containing 20 mmol·L-1 sodium heptanesulfonate, adjusted to pH 2.80 with phosphoric acid) (at a ratio of 45:55) and the resolution of D-malic acid and L-malic acid derivatization products reached 1.7. The proposed method possesses the advantages of simple operation, mild conditions, stable derivatization products and low cost. Also it gave better separation and was more accurate than previous methods.
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
Food Analytical Methods
·
2013
·Vol. 7
·期 7
·1400-1406
·
IF 1.969
Liu Tenghao,Jiang Zi-Tao,Li Rong,Tan Jin
This paper aims at establishing a rapid method for simultaneous separation and determination of the sweeteners including cyclamate, acesulfame, and aspartame in beverages by titania-based reversed-phase high-performance liquid chromatography. The chromatographic conditions were as follows: a titania Sachtopore-RP C18 column (250 × 4.6 mm; 5 μm) as a separation column, a mixture of water and methanol at a volume ratio of 95:5 containing 1.0 % phosphate acid used as mobile phase, flow rate of 1.0 mL min −1 , and the detection wavelength was 205 nm. The linear ranges of cyclamate and aspartame were 0.02–8.0 mg mL −1 with limits of detection (LODs) of 16.35 and 19.56 μg mL −1 , respectively, and their limits of quantitation (LOQs) were 55.50 and 68.50 μg mL −1 , respectively. The recoveries of cyclamate were between 93.52 and 103.54 %. The recoveries of aspartame were between 93.31 and 102.63 %. The linear range of acesulfame was 0.125–50 μg mL −1 with LOD of 0.08 μg mL −1 and LOQ of 0.25 μg mL −1 . The recoveries of acesulfame were between 94.34 and 103.21 %. Relative standard deviation ( n = 8) for all determinations was less than 0.72 %.
研究领域:
分析化学
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食品科学
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DOI
高影响因子
RSC Advances
·
2021
·Vol. 11
·期 37
·23002-23009
·
IF 3.361
Peng Jin,Kai Yang,Ruining Bai,Mei Chen,Shilin Yang,Kebo Fu,Jieli He
Microcystin-LR (MC-LR) generated by cyanobacteria is a kind of potent hepatotoxin, which poses a considerable threat to human health. In the research field of MC-LR removal, the quantitative analysis in a wide concentration range of samples is inevitable. In this paper, we presented the pseudo united use of an Ultra Performance Liquid Chromatography Mass Spectrometry (UPLC-MS) and High Performance Liquid Chromatography system with a Variable Wavelength Ultraviolet Detector (HPLC-VWD) approach to detect MC-LR. The UPLC-MS system was applied to determine MC-LR in trace concentration because of its high sensitivity. However, it is generally believed that the determination of high concentration samples by UPLC-MS will cause problems such as inaccurate quantification and contamination of ion sources. In consequence, the HPLC-VWD was employed to determine the high concentration of MC-LR. The sensitivity, precision and accuracy of the two methods were compared in detail. The linear ranges of UPLC-MS and HPLC-VWD methods were from 0.08 to 10 μg L−1 and 1 to 5000 μg L−1, respectively. The detection and quantification limits of UPLC-MS were 0.03–0.05 μg L−1 and 0.08 μg L−1, and the corresponding two values of HPLC-VWD were 0.6 and 1.0 μg L−1. The recoveries of UPLC-MS and HPLC-VWD were 88.5–106.7% and 98.7–101.6%, with the relative standard deviations of 3.72–5.45% and 0.38–1.69%, respectively. The potential adsorption properties of MC-LR on filter membranes with diverse materials and pore sizes were evaluated and the negative results were obtained. The detection of MC-LR by UPLC-MS was free from matrix effects. The presented UPLC-MS and HPLC-VWD methods were used to analyze the water samples from Erhai Lake, which is located in Dali, Yunnan, China. The results of UPLC-MS analysis indicated that the MC-LR was only identified in water samples of Shuanglang Bay and Xier River, with concentrations of 0.120 and 0.303 μg L−1, whereas MC-LR was not detected by HPLC-VWD.
研究领域:
环境科学
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毒理学
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分析化学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2023
·Vol. 37
·期 4
·e5580
·
IF 1.8
Rathnakar Nathi,Leela Prasad Kowtharapu,Siva Krishna Muchakayala,Naresh Konduru
A nonsteroidal drug called flurbiprofen (FBN) has analgesic, anti-inflammatory and antipyretic activity. Currently the determination of FBN in cataplasm does not have any pharmacopeial method. However, the drug substance, tablet and ophthalmic solution formulations do have pharmacopeial methods. The development and validation of an accurate, precise and stability-indicating analytical method for the determination of FBN in cataplasm formulations is reported. The gradient method was employed for the quantification of FBN in the presence of internal standards such as biphenyl. A nonpolar separation phase (C 18 , 250 × 4.6 mm, 5 μm Inertsil column; GL Sciences) was used. The optimal flow rate, column oven temperature, injection volume and detector wavelengths were 1.0 ml/min, 40°C, 20 μl and 245 nm, respectively. Mobile phase A was a mixture of water and glacial acetic acid (30:1 v/v) pH adjusted to 2.20 with glacial acetic acid or 1 m NaOH; mobile phase B was methanol (100%). The gradient elution program was [time (min)/% B]: 5/60, 20/70, 25/70, 30/60 and 40/60. The obtained RSDs for the precision and intermediate precision were 0.7 and 0.5%. The percentage recovery ranged from 99.2 to 100.4%. The linear regression coefficient >0.9996 indicates that all peak responses were linear with the concentration. The sample and standard solutions were stable for up to 24 h on the benchtop and in the refrigerator. The critical peaks were well separated from the generated peaks owing to forced degradation, including diluent and placebo peaks. The method validation data and quality by design-based robustness study results indicate that the developed method is robust and fit for routine use in the quality control laboratory. The proposed method is specific, accurate and precise, and the quality by design utilized the first method for the determination of FBN in cataplasm formulations. Transdermal patches and gels have low extraction capacity and this method is applicable for quantification.
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
LUMINESCENCE
·
2016
·Vol. 32
·期 1
·4-10
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IF 1.452
Dan Liu,Jingdong Peng,Shaopu Liu,Mingqiong Zhou,Jing Zhang,Aiping Li
A highly selective and sensitive method of reversed phase high-performance liquid chromatography (RP-HPLC) coupled with resonance Rayleigh scattering (RRS) was developed for the determination of procaine, bupivacaine and tetracaine. Separation of three local anaesthetics was achieved at 35 °C on a C 18 column. The mobile phase was 30: 70 (v/v) acetonitrile/triethylamine–phosphoric acid buffer (pH 2.9) at flow rate of 0.3 mL/min. The RRS detection was conducted by taking advantage of the strong RRS enhancement of the local anaesthetics with erythrosine reaction in an acidic medium. Under optimum conditions, the limit of detection (S/N = 3) values were in the range of 2.4–11.2 ng/mL. Recoveries from spiked human urine samples were 95.8%–104.5%. The proposed method applied to the determination of local anaesthetics in human urine achieved satisfactory results. In addition, the mechanism of the reaction is fully discussed. Copyright © 2016 John Wiley & Sons, Ltd.
研究领域:
分析化学
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药学
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DOI
PubMed
高影响因子
CHROMATOGRAPHIA
·
2022
·Vol. 86
·期 1
·55-62
·
IF 2.213
Zhang Caiyu,Li Wei,Ning Baoming
This study aimed to develop and validate a high-performance liquid chromatography system combined with a single-quadrupole Dalton mass detector for the separation and determination of pidotimod (( R )-3-[( S )-(5-oxo-2-pyrrolidinyl)carbonyl]-thiazolidine-4-carboxylic acid) and its three isomers. The separations were achieved using a Lux Amylose-1 column operated at 40 °C using acetonitrile/0.1% trifluoroacetate (TFA) and isopropanol/0.1% TFA (90:10, v / v ). The enantiorecognition mechanism was also elucidated using the ORCA 5 program. Four isomers were successfully separated with a resolution (Rs) > 1.5, with the method showing satisfactory linearity in the ranges of 0.2 to 3.5 μg·mL −1 ( S,R; S,S ) and 0.5 to 3.5 μg·mL −1 ( R,S; R,R ), along with good specificity, accuracy, and precision. Further, three batches of pidotimod oral solutions were evaluated and the S,S -isomer in each batch was detected at about 0.05%. Moreover, computational evaluations suggested that the sorbent-analyte interactions of amylose tris(3,5-dimethylphenycarbamate) can be used to successfully interpret and even predict the chromatographic separation results. The validated method showed high sensitivity and can potentially be used to analyze the isomer impurities of raw materials for quality control purposes.
研究领域:
药物分析
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色谱技术
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质量控制
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DOI
高影响因子
Food Analytical Methods
·
2021
·Vol. 14
·期 7
·1345-1358
·
IF 3.366
Wei Yihua,Zhang Jinyan,Qiu Shuyan,Huang Qingqing,Yuan Linfeng,Chen Liumeng,Dai Tingcan,Tu Tianhua,Zhang Biaojin,Yan Han,Li Weihong
A simple, rapid, and accurate method for determination of selenocystine (SeCys 2 ), methyl selenocysteine (MeSeCys), selenourea (SeUr), selenite (Se(IV)), selenotmethionine (SeMet), and selenate (Se(VI)) in grain crops was developed, based on the coupling of ion-pair reversed-phase high-performance liquid chromatography (IP-RP-HPLC) and ultraviolet irradiation hydride generation atomic fluorescence spectrometry (UV-HG-AFS). The conditions of IP-RP-HPLC-UV-HG -AFS were studied. The conditions of the pretreatment sample, such as types and dosage of proteinases, were investigated. The detection limits (LODs) for six Se species were between 0.77 and 1.77 μg·L −1 . Then, the proposed method has been successfully used to analyze selenium (Se) species in Se-enriched rice paddy ( Oryza sativa L. ), soybean ( Glycine max (Linn.) Merr. ), and sweet potato ( Ipomoea batatas (L.) Lam. ) with foliar application of sodium selenite solution. SeMet was the major Se spices in Se-enriched grain crops, ranged from 77–90% of the total Se contents. The capabilities of Se enrichment were relatively larger differences in three-grain corps as follows: soybean > rice paddy > sweet potato.
研究领域:
植物学
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分析化学
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营养学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2024
·
IF 1.5
Zhang Chenxia,Wu Zeyi,Qiu Meiyan,Li Yanhua,Wang Zhongqing,Fan Xiaomei,Cai Shaoyu,Rao Wanbing
The difficulty on determination of high boiling point solvents, always exist due to their low vapor pressure in headspace (HS) vial. What’s worse, the commonly used GC diluents, such as N, N-dimethylacetamide, 1,3-dimethyl-2-imidazolidinone, dimethyl sulfoxide, N, N-dimethylformamide and N-methylpyrrolidone are often remained in HS instrument after frequent injection into HS, thus would result in terrible positive interference problem. In this work, a fast and sensitive HPLC method in combination with a sample precipitation method, was proposed for the determination of above five high boiling point solvents in drug substances within 14.5 min. The final method was validated with regard to limit of detection and limit of quantitation, precision, linearity and accuracy in accordance with ICH Q2 (R1). Finally, the proposed strategy was successfully applied for the analysis of high boiling point solvents used in three active pharmaceutical ingredients. The established generic strategy would provide another choice for the determination of high boiling point solvents in pharmaceuticals.
研究领域:
分析化学
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药学
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产品关联
DOI
PubMed
高影响因子
SCIENCE OF THE TOTAL ENVIRONMENT
·
2023
·
IF 9.8
Wenhao Guan,Zhijia Fang,Yinyan Chen,Yongbin Li,Zhilan Peng,Lijun Sun,Qi Deng,Ravi Gooneratne
As one of the most accumulative toxic heavy metals, cadmium (Cd) poses a major threat to human health. Bacterial siderophores, as small molecules with metal-absorbing ability, have great potential activity for Cd-reduction. In this study, the siderophore-producing bacterialstrain FCH-CR2 was isolated from a high-Cd contaminated soil using the CAS method. Leclercia adecarboxylata was identified through 16S rRNA sequence, homology analysis, colony morphology, physiological and biochemical tests. A siderophore, catechol type 2,3-dihydroxy-N-benzoyl- l -serine (DHBS) secreted by FCH-CR2, was purified using RP-HPLC and identified by LC-MS/MS. Intraperitoneal injection of DHBS significantly increased fecal Cd levels, and reduced Cd accumulation in organs. In density flooding theory (DFT) analysis, DHBS may bind to Cd via the hydroxyl site on the benzene ring. Besides, the isothermal titration calorimetry (ITC) assay revealed that the formation of Cd-DHBS is a spontaneous and endothermic reaction with ΔG = −21.4 kJ/mol and ΔH = 1.51 ± 0.142 kJ/mol.
研究领域:
环境科学
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微生物学
·
化学
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DOI
PubMed
高影响因子
JOURNAL OF FOOD SCIENCE
·
2024
·
IF 3.2
Weijing Wu,Libo Wang,Ju Qiu,Ziyuan Zhuang,Fei Qin,Qianglai Tan,Yanling Wang,Lanlan Wu
Tartary buckwheat, a protein-rich pseudocereal with anti-diabetic effects, has not yet been fully explored as a source of dipeptidyl peptidase-IV (DPP-IV) inhibitory peptides. This study aims to discover novel DPP-IV inhibitory peptides from tartary buckwheat protein (TBP). Five hydrolysis methods were employed, with simulated gastrointestinal digestion (SGID) releasing the most active DPP-IV inhibitory hydrolysates, showing both the highest degree of hydrolysis (22.66 ± 1.12%) and inhibition activity (41.81 ± 1.52% at 1.25 mg/mL). In addition, ultrafiltration enriched the <3 kDa fraction with the highest inhibitory rate, and further purification using reverse-phase high-performance liquid chromatography concentrated the DPP-IV inhibitory peptides in the first fraction (F1). Nano liquid chromatography-tandem mass spectrometry analysis identified 10 new peptides in F1, among which the peptide Leu-His-Ile-Val-Gly-Pro-Asp-Lys (LHIVGPDK) exhibited the strongest inhibitory effect, with an IC 50 value of 1.61 mM. Kinetic studies revealed that LHIVGPDK acts as a mixed-type inhibitor, and molecular docking indicated that it inhibits DPP-IV by forming stable complexes through five types of interactions, with hydrogen bonds playing a key role. This study underscores TBP's DPP-IV inhibitory potential and anti-diabetic properties, reinforcing the value of tartary buckwheat as a beneficial food for diabetes management. Practical Application This research identified new peptides from Tartary buckwheat protein that effectively inhibit DPP-IV, an enzyme associated with diabetes management. These findings suggest potential applications in developing functional foods to help control hypoglycemia.
研究领域:
食品科学
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营养学
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生物化学
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药理学
·
糖尿病管理
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产品关联
DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF FOOD SCIENCE AND TECHNOLOGY
·
2020
·Vol. 56
·期 1
·138-147
·
IF 2.773
Jun Feng,Yi-Long Ma,Ping Sun,Kiran Thakur,Shaoyun Wang,Jian-Guo Zhang,Zhao-Jun Wei
Summary Enzymatically derived peptides from different proteins have displayed the potential to provide health benefits. Present research aims to obtain the functional peptides and improve the economic value of camellia seed cake via enzymatic hydrolysis. Camellia seed cake protein hydrolysates (CSCPH) prepared with alcalase demonstrated higher α-glucosidase inhibitory activity. After ultrafiltration, the α-glucosidase inhibitory activity of different components was compared. The component (CSCPH-IV) with the highest activity was selected for further separation and purification. The peptides were purified using reverse-phase high-performance liquid chromatography (RP-HPLC) twice and identified as GHSLESIK, GLTSLDRYK and SPGYYDGR by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Subsequently, the preliminarily inhibitory effect of these peptides on α-glucosidase activity was demonstrated by the molecular docking model. These results showed that three novel peptides isolated from the hydrolysates of camellia seed cake have the potential to be used as anti-diabetic compounds for the development of functional foods.
研究领域:
食品科学
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药理学
·
生物化学
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DOI
高影响因子
Scientific Reports
·
2017
·Vol. 7
·期 1
·1-12
·
IF 4.259
Jiang Bin,Zhang Xiaoqing,Yuan Yongqiang,Qu Yuxiao,Feng Zhibiao
An aqueous two-phase system (ATPS) consisting of poly(ethylene glycol-ran-propylene glycol) monobutyl ether (UCON)/phosphate was developed for the separation of the antioxidant peptides from pepsin hydrolysate of Whey Protein Isolate (WPI). The efficiency of the separation was evaluated based on the DPPH radical scavenging activity, ABTS radical scavenging activity and ferric reducing antioxidant power (FRAP) of the separated peptides. The effects of some parameters on the partition of antioxidant peptides were investigated. An efficient separation of antioxidant peptides was achieved using ATPS with pH of 4.0, 4 mL of UCON solution (40%, w / w ), 4 mL of KH 2 PO 4 solution (15.5%, w / w ), 2 mL of WPI hydrolysate and 0.40 g/10 mL of NaCl. Reversed-phase high-performance liquid chromatography (RP-HPLC), amino acid analyzer and matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) were used to characterize the purified peptides separated by the ATPS. The peptides in top phase were less polar than those in bottom phase. More antioxidative and hydrophobic amino acids were extracted to the top phase of ATPS, and the peptides with the amino acid sequences with antioxidant activities moved to the top phase as well. In conclusion, antioxidant peptides were successfully separated from the WPI hydrolysate by UCON/phosphate ATPS.
研究领域:
生物化学
·
食品科学
·
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）