Analytical Methods
·
2018
·Vol. 10
·期 41
·4978-4984
·
IF 2.073
Xing Huang,Kaipeng Zhang,Yanli Tong,Yongsheng Zhong,Zuanguang Chen
In this study, a gradient reverse phase high performance liquid chromatography combined with a capacitively coupled contactless conductivity detection (RP-HPLC-C4D) method for simultaneous determination of phospholipid and fatty glyceride in liposome was developed. After saponification, the fatty glyceride and two types of phospholipids were transformed into octanoic acid, palmitic acid and erucic acid, respectively, which were then separated and detected by RP-HPLC-C4D. The results showed good linearity in the range of 20–1000 μg mL−1 for octanoic acid and erucic acid and 10–1000 μg mL−1 for palmitic acid. The LODs of octanoic acid and palmitic acid reached 2.5 μg mL−1, and 10 μg mL−1 for erucic acid. The average recoveries of octanoic acid, palmitic acid and erucic acid were 100.2%, 102.9% and 101.4% (n = 9), respectively. The developed method could be effectively applied in the quality control and stability monitoring of liposome.
研究领域:
分析化学
·
药剂学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2015
·Vol. 54
·期 3
·353-360
·
IF 1.363
Zhou Yuxia,Zhou Fan,Yan Fei,Yang Feng,Yao Yuxian,Zou Qiaogen
Eleven potential impurities, including process-related compounds and degradation products, have been analyzed by comprehensive studies on the manufacturing process of clevidipine butyrate. Possible formation mechanisms could also be devised. MS and NMR techniques have been used for the structural characterization of three previously unreported impurities (Imp-3, Imp-5 and Imp-11). To separate and quantify the potential impurities in a simultaneous fashion, an efficient and advanced RP-HPLC method has been developed. In doing so, four major degradation products (Imp-2, Imp-4, Imp-8 and Imp-10) can be observed under varying stress conditions. This analytical method has been validated according to ICH guidelines with respect to specificity, accuracy, linearity, robustness and stability. The method described has been demonstrated to be applicable in routine quality control processes and stability evaluation studies of clevidipine butyrate.
研究领域:
药物化学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD QUALITY
·
2022
·
IF 3.2
Yingqi Chen,Chonggao Hu,Jiaojiao Xu,Xiaodong Pan,Baifen Huang
In this paper, we built a method of verifying the 4 retinols of vitamin A and 8 tocopherol isomers of vitamin E in the food industry based on RP-HPLC-PDA-FLR. The effect of laboratory light conditions on the target components was considered for the first time, and it was found that the loss rate of the target components was the smallest in the case of a white laboratory bench with red or LED light in the dark room. There was no finding of extraction recoveries of the target components with a significant difference under different saponification conditions. Meanwhile, it was found that using ethyl acetate/n-hexane mixed solvent as the extraction solvent could ensure the effective extraction of the target components. Finally, baseline separation of 12 components was achieved within 45 min using the C30 column. With the help of methodological verification, we found that the recovery rate ranged from 76.45% to 93.52%, and RSD was between 0.19% and 12.99%; the Limit of Detection minimum value was 0.01 mg/100 g and the Limit of Quantitation minimum value was 0.03 mg/100 g. The detection method was successfully applied to the distribution detection of 4 kinds of retinols and 8 kinds of vitamin E in egg and dairy products and provided technical support for the accurate nutritional evaluation of vitamin A and vitamin E.
研究领域:
食品科学
·
分析化学
✓ 已验证
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
·
分析化学
✓ 已验证
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
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2014
·Vol. 6
·期 5
·1563-1568
·
IF 1.938
Huang Yang,Li Kang,Shao Hui Kai,Liu Sheng Quan,Xiang Fei Jun
A method using molecularly imprinted solid-phase extraction combined with RP-HPLC-UV was developed for determination of liquiritin (LQR) in rat plasma after oral administration of Compound Liquorice Tablets (CLTs). To this end, molecularly imprinted polymers were prepared by in situ polymerization, using LQR as the template, acrylamide as the functional monomer, and ethylene glycol dimethacrylate as the crosslinker, whose solid-phase extraction properties for liquiritin were evaluated by HPLC-UV. The enrichment and extraction recovery were investigated in the study after the extraction procedure was optimized. The recovery was larger than 85.0% and the RSD was less than 10.0%. The calibration curve was expressed as y = 16 004x − 1.864 (r = 0.996) with a linear range of 0.007–1.683 μg mL−1. Besides, the Tmax was 0.5 h for liquiritin and the Cmax was 0.8 μg mL−1 after oral administration of compound liquorice tablets. In addition, the pharmacokinetic parameters were calculated using a two-compartment model. The results indicated that the monolithic polymer pipette presented a good extraction efficiency for liquiritin. At the same time, the results indicated that the index components could basically reveal the pharmacokinetic behavior. This study was aimed to explore an approach that could be applied to promulgate the pharmacokinetics and provide more information for clinical applications.
研究领域:
药理学
·
分析化学
·
生物医学工程
✓ 已验证
产品关联
DOI
高影响因子
THERAPEUTIC DRUG MONITORING
·
2025
·
IF 2.4
Dong Zhonghua,Wang Peng,Cui Xueyan,Liu Jinjuan,Shi Haiyan,Yang Yilei,Xu Jingya,Yi Qiaoyan
Background: Perampanel (PER), a novel antiepileptic drug, exhibits high protein binding. Given the drug's susceptibility to various factors, including drug interactions, and the considerable variability in blood concentrations among individuals, solely measuring the total plasma concentration of PER may not provide comprehensive insights. This study aimed to establish an HPLC-FLD method to quantify both total and free PER in clinical samples. Methods: Analysis of total PER involved a straightforward sample preparation process involving plasma protein precipitation. Plasma samples were ultrafiltered to isolate the free portion of PER. Chromatographic separation was achieved on an InertSustain C18 column at a 1-mL/min flow rate using a gradient of acetonitrile and aqueous sodium acetate buffer at pH 4.4. Results: Calibration curves for total and free PER in plasma exhibited excellent linearity over the concentration ranges of 10–3000 and 0.5–100 ng/mL, respectively. The method was applied to analyze blood samples from patients with epilepsy quantitatively; the total concentration of perampanel in the plasma of the patients was in the range of 90.45–563.39 ng/mL, whereas the free concentration was in the range of 1.82–15.29 ng/mL. The plasma protein binding ratio of perampanel was normally between 97.09% and 99.29% and decreased in cases of hypoproteinemia. Conclusions: The method was rigorously validated for selectivity, accuracy, precision, and stability in accordance with established FDA and EMA guidelines. The developed method enables the rapid and accurate quantification of both total and free PER concentrations in the plasma of patients with epilepsy, offering technical support for its subsequent clinical application.
研究领域:
临床药理学
·
分析化学
·
神经病学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2012
·Vol. 4
·期 10
·3471-3477
·
IF 1.547
Xu Han,Lianghui Cao,Heyong Cheng,Jinhua Liu,Zigang Xu
Ion-pair reversed phase high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (RP-HPLC-ICP-MS) has been used to determine two inorganic iodine species (I− and IO3−) and two organic iodinated amino acids (MIT and DIT) in seaweed and seawater samples within 5 min. The mobile phase used for a reversed phase C18 column was as follows: 2.0 mM tetraethylammonium hydroxide, 10 mM L-phenylalanine and 1% methanol (pH 8.9). Values of 1.5 mL min−1 for the flow rate of the mobile phase and 25 °C for the column temperature were selected for rapid separation of iodine species. The detection limits for IO3−, I−, MIT and DIT were 0.061, 0.052, 0.079 and 0.24 μg L−1, each, and the repeatabilities of peak height and peak area (20 μg L−1 for iodide and iodate, 40 μg L−1 for MIT, 100 μg L−1 for DIT) were all lower than 4%. Under the optimized conditions, the proposed method was successfully applied for the speciation analysis of iodine in seaweed and seawater samples. Recoveries of IO3−, I−, MIT and DIT in seaweed and seawater samples were between 90 and 110%. All results prove its advantages including high sensitivity, environmentally friendly, low time consumption, which are beneficial for routine analysis of iodine speciation in environmental and food fields.
研究领域:
分析化学
·
环境科学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
Analytical Methods
·
2012
·Vol. 4
·期 4
·1012-1018
·
IF 1.547
Xiaojie Liu,Yuzhi Wang,Jinhuan Kong,Chan Nie,Xiao Lin
Eight types of ionic liquid (IL) were synthesized in this paper, and ionic liquids-based microwave-assisted extraction (ILs-MAE) technique was used to extract quercetin from the Chinese herbal medicine Toona sinensis. Several significant operating parameters were optimized by a series of single factor experiments and orthogonal design L9 (34) experiments in this work. Compared with liquid-based maceration extraction (ILs-ME), liquid-based heat extraction (ILs-HE) and liquids-based ultrasound-assisted extraction (ILs-UAE), the optimized approach of ILs-MAE technique cost the shortest time but afforded the highest extraction amount. Moreover, reversed phase high performance liquid chromatography (RP-HPLC) with ultraviolet detection (UV-DAD) was employed for the analysis. The results show that the amount of quercetin extracted by [Bmim]Br was 182.78 mg g−1 with RSD 1.02%. The developed approach is linear between concentrations from 15.20 mg L−1 to 213.2 mg L−1 of quercetin and the regression coefficient (R) was 0.9992. The recoveries of quercetin extracted by these four methods were 95.07%–105.8% with RSDs lower than 3%. Furthermore, the change of the microstructure and chemical structure of the sample before and after different extraction procedures were researched, respectively. Because of the remarkable dissolving capacity of ILs aqueous solution and the obvious destruction on sample surface microstructures during ILs-MAE process, ILs-MAE technique got the highest extracted amount. With the help of LC-MS, we can further confirm that Toona sinensis do contain the active ingredient of quercetin and ILs had no interference of quercetin.
研究领域:
药学
·
分析化学
✓ 已验证
DOI
高影响因子
ANALYTICAL SCIENCES
·
2018
·Vol. 34
·期 3
·283-289
·
IF 1.355
Xiao-Lin SHAN,Xiao-Ting LIU,Can GONG,Xu XU
The complexity of triacylglycerols (TAGs) in edible oils is largely due to the many similar unsaturated TAG compounds, which makes profiling TAGs difficult. In this study, precolumn derivatization with bromine (Br2) was used to improve the separation and detection sensitivity of TAGs in edible oils by RP-HPLC. Oil samples dissolved in n-hexane and TAGs were derived by reaction with a Br2–CCl4 (1:1, v/v) solution for 3 h at room temperature. The derivate product solution was stable and was best separated and detected by RP-HPLC using a C18 column, with a mobile phase of methanol–n-hexane (91.5:8.5, v/v) at 25°C. A detection wavelength of 230 nm was used. The results showed that the approach enabled the separation and detection of more similar TAGs by RP-HPLC. The method was applied to profile 20 types of edible oil, and the results presented the differences in the TAG profiles of various edible oils, which may be useful in the identification of edible oils.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Current Analytical Chemistry
·
2017
·Vol. 13
·期 4
·317-324
·
IF 1.306
Guo Yuanheng,Zhao Bing
Objective: A comprehensive monosaccharide quantifying method was developed in this article. Monosaccharides (including glucose, arabinose, galacturonic acid, galactose, mannose, rhamnose and xylose) were analyzed by RP-HPLC-DAD method. Meanwhile, mannitol and fructose were calculated
based on peak areas obtained by HPIEC-RID and corresponding data obtained by RP-HPLC-DAD. Monosaccharide compositions of CDSC were analyzed, nine kinds of monosacchardes (glucose, arabinose, galctose, galacturonic acid, mannose, rhamnose, xylose, fructose and mannitol) in were quantified.
Background: Cistanche deserticola Y. C. Ma, is a perennial holoparasite and mainly distributed in the desert region of northwestern China. It reported that C. deserticola soluble carbohydrate (CDSC) could prompt lymphocyte proliferation, modulate immunity, inhibit type 2 diabetes, anti-inflammation.
For these reasons, it is very appealing to researchers to have a convenient method for monosaccharides analysis of the CDSC. However, previous researches have neglected the faultiness in monosaccharide composition analysis. Therefore, in this study we will focus on establishing a quantifying
method of monosaccharides possibly found in C. deserticola. Methods: Soluble carbohydrates were hydrolyzed with trifluoroacetic acid, monosaccharides were labeled with 1-phenyl-3-methyl-5-pyrazolone (PMP), separated by HPLC system equipped with C18 column and detected with DAD (RP-HPLC-DAD).
RP-HPLC-DAD method was used for quantitative analysis of glucose, arabinose, galacturonic acid, galactose, mannose, rhamnose and xylose. Meanwhile, hydrolyzates were separated by HPIEC system equipped with aminex HPX-87H ion exclusion column and detected by refractive index detector (HPIEC-RID).
The quantity of mannitol and fructose can be calculated based on peak areas obtained by HPIEC-RID and corresponding data obtained by RP-HPLC-DAD. Results: Utilizing this method, monosaccharide compositions of CDSC with different molecular weight (CDCSA, CDCS-B, CDCS-C and CDCS-D) were
analyzed, nine kinds of monosacchardes (glucose, arabinose, galctose, galacturonic acid, mannose, rhamnose, xylose, fructose and mannitol) in were found. Conclusion: Fructose and mannitol, which are abundant present in C. deserticola, cannot be analysis by normally PMP modify method,
therefore, a comprehensive quantitative analysis method was developed in this research. Galacturonic acid was found out in macro-molecular polysaccharides from C.deserticola, which was not reported before. Galactose and galacturonic acid mainly exist in macro-molecular polysaccharide. Fructose
and mannitol mainly exist in mini-molecule or exist in free form.
研究领域:
植物化学
·
分析化学
✓ 已验证
DOI
高影响因子
SEPARATION AND PURIFICATION TECHNOLOGY
·
2015
·
IF 3.091
Xiao-Hui Yao,Dong-Yang Zhang,Ming-Hui Duan,Qi Cui,Wen-Jing Xu,Meng Luo,Chun-Ying Li,Yuan-Gang Zu,Yu-Jie Fu
A group of green solvent named polyols-based deep eutectic solvents (PDES) combined with microwave assisted extraction (MAE) was first successfully applied in extracting phenolic compounds from pyrola. A series of PDES with mixing different ratios choline chloride (ChCl) to different polyols were investigated for extraction, and ChCl/1,4-Butanediol (1/4) was found to be the suitable extraction solvent. MAE was more effective than heat-stirring extraction and ultrasonic assisted extraction with PDES. The extraction parameters were optimized by BBD test combined with response surface methodology. The optimal extraction conditions were 30% of water in ChCl/1,4-Butanediol (1/4) at 70 °C for 20 min and liquid/solid ratio 10 mL/g. Moreover, RP-HPLC-UV was developed for the determination of five main active components in pyrola. This method exhibited satisfactory linearity ( R 2 > 0.999), precision (RSD < 4.03%) and recovery (96.17–103.25%). Sample analysis showed that the contents of hyperin, 2′-O-galloylhyperin, quercitrin, quercetin-O-rhamnoside and chimaphilin in pyrola were 1.627, 4.958, 0.041, 0.089 and 0.349 mg/g, respectively. These results revealed that PDES would be promising green solvents for analytical sample preparation from plant herbs.
研究领域:
植物化学
·
分析化学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）