JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2022
·
IF 4.52
Yan Zhang,Cuiling Cao,Zhiwei Yang,Guangqun Jia,Xiaomao Liu,Xuemin Li,Zongyan Cui,Adan Li
Propolis is rich in flavonoids and phenolic acids , which has strong antioxidant capacity . Two methodologies for simultaneous determination of 20 phenolic compounds in propolis by HPLC-UV and HPLC-MS/MS were developed. The sample extraction and chromatographic separation conditions, and ultraviolet detection wavelength, as well as mass spectrometry parameters were selected and optimized. Under the optimized conditions, good linearities ( R 2 ≥0.998) were obtained for all analytes. The limits of quantification (LOQs) of the proposed methods by HPLC-UV and HPLC-MS/MS for all analytes were in the range of 0.02–0.1 mg/g and 0.05–0.2 mg/g, respectively, and the recoveries were in the range of 95.4 %− 109.5 % and 94.0 %− 106.8 % with the relative standard deviations (RSDs) in the range of 1.1 %− 7.5 % and 0.4 %− 11.1 %, respectively. The proposed methods were applied for the determination of 20 phenolic compounds in 13 propolis samples collected from China and Brazil. The detection results of the two methods are almost consistent with each other, indicating that both methods are applicable, and the inter-confirmation of the two methods can improve the accuracy of the determination of phenolic components in propolis.
研究领域:
植物化学
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分析化学
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药学
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DOI
高影响因子
RSC Advances
·
2021
·Vol. 11
·期 48
·30102-30108
·
IF 3.361
Setareh Rostami-Javanroudi,Masoud Moradi,Kiomars Sharafi,Nazir Fattahi
In the present research, several novel and natural hydrophobic deep eutectic solvents (DESs) were prepared using methyltrioctylammonium chloride (MTOAC) as the hydrogen bond acceptor (HBA) and different types of straight chain alcohols as hydrogen bond donors (HBDs). One of the DESs composed of MTOAC and n-butanol was advantageously used to develop a vortex-assisted liquid phase microextraction (VALPME) method combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) for the determination of common acaricides in fruit juice samples. Several important parameters influencing extraction efficiency were investigated and optimized, including the type and volume of DES, sample solution pH, effect of salt addition and, extraction and vortex time. Under optimal experimental conditions, the method showed good linearity with the correlation coefficients (R2) of 0.9986–0.9991 in the linear range of 2–300 μg L−1, low limits of detection of 0.5–1 μg L−1 and acceptable extraction recoveries in the range of 85–93%. The proposed method was successfully applied for the extraction and preconcentration of trace acaricides in real fruit juice samples, and the results demonstrated the potential of the synthesized DESs for the extraction and determination of contaminants in aqueous samples.
研究领域:
分析化学
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食品安全
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产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2019
·Vol. 12
·期 2
·141-148
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IF 2.378
Xue Ren,Man He,Beibei Chen,Bin Hu
Herein, magnetic porous organic polymers (MOPs) prepared via an azo coupling reaction in water under mild conditions are evaluated for the extraction of seven cardiovascular drugs, including xylocaine, metoprolol, mexiletine, labetalol, propranolol, carvedilol and propafenone, from human urine samples for the first time. The extraction mechanisms are assumed to be electrostatic interaction and π–π stacking. The MOPs exhibited fast adsorption/desorption time (13 min) and high enrichment factors (315–365-fold) for target analytes. Based on this, a method coupling magnetic solid phase extraction with HPLC-UV detection was developed for the analysis of cardiovascular drugs. Under the optimized conditions, the LODs (S/N = 3) were in the range of 0.06–0.57 μg L−1 with an RSD (n = 5) of 4.3–8.6%, and the linear range was 0.2–200 μg L−1 for propranolol, 2–200 μg L−1 for metoprolol, and 0.5–200 μg L−1 for the other five analytes. The developed method was applied for the analysis of cardiovascular drugs in urine samples with recoveries of 89.0–112%. In order to further evaluate the application potential of this method, real-time monitoring of metoprolol in urine samples collected from volunteers treated with metoprolol tablets was performed. The proposed method is simple, fast, and sensitive and has good potential in the monitoring of cardiovascular drugs in competitive sports and clinical analysis.
研究领域:
分析化学
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药理学
✓ 已验证
产品关联
DOI
高影响因子
BMC Complementary Medicine and Therapies
·
2020
·Vol. 20
·期 1
·1-10
·
IF 0
Li Hong-Ying,Fang Jiang-Ji,Shen Hua-Dan,Zhang Xue-Qiong,Ding Xiao-Ping,Liu Jun-Feng
Background Quantitation analysis and chromatographic fingerprint of multi-components are frequently used to evaluate quality of herbal medicines but fail to reveal activity of the components. It is necessary to develop a rational approach of chromatography coupled with activity detection for quality assessment of herbal medicines. Methods An on-line HPLC-ultraviolet detection-2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) free radical scavenging (HPLC-UV-ABTS) method was developed to obtain the chromatographic fingerprints and ABTS +• inhibition profiles (active fingerprints) of Rehmanniae Radix (Dihuang) and Rehmannia Radix Praeparata (Shu Dihuang). Eighteen compounds showing ABTS +• inhibition activity were identified by HPLC-fourier-transform mass spectrometry (HPLC-FTMS). Verbascoside was used as a positive control to evaluate the total activities of the samples and the contribution rate of each compound. The similarities of the chromatographic and active fingerprints were estimated by the vectorial angle cosine method. Results The results showed that the HPLC-UV-ABTS method could efficiently detect antioxidant activity of the herbal medicine samples. The antioxidants were different between the two herbs and several new antioxidants were identified in Shu Dihuang. A function equation was generated in terms of the negative peak area (x) and the concentrations of verbascoside (y, μg/mL), y = 2E-07 × 4 - 8E-05 × 3 + 0.0079 × 2 + 0.5755x + 1.4754, R 2 = 1. Iridoid glycosides were identified as main antioxidants and showed their higher contributions to the total activity of the samples. The total contributions of the three main active components in the Dihuang and Shu Dihuang samples to the total activity, such as echinacoside, verbascoside and an unknown compound, were 39.2–58.1% and 55.9–69.4%, respectively. The potencies of the main active components in the Shu Dihuang samples were two to ten times those in the Dihuang samples. Similarity values for S12 in the chromatographic fingerprints and S03, S12 and P03 in the active fingerprints were less than 0.9. The three batches of samples might show their different quality with the other samples. Conclusions The results suggested that the combination of “quantity-effect” research strategy and the HPLC-UV-ABTS analysis method could comprehensively evaluate the active components and quality of Dihuang and Shu Dhuang.
研究领域:
中药学
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分析化学
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药理学
✓ 已验证
产品关联
DOI
PubMed
RSC Advances
·
2019
·Vol. 9
·期 44
·25797-25804
·
IF 3.049
Shunli Ji,Hongbin Gao,Xingya Xia,Feng Zheng
Benzyl halides, widely used as alkylation reagents in drug synthesis, are potential genotoxic impurities (PGTIs) required to be controlled at trace levels. However, the existing analytical methods for benzyl halides often suffer from matrix interferences or low derivatization efficiency of benzyl chlorides. In this paper, a simple derivatization HPLC-UV method was developed for the analysis of these residual trace benzyl halides in drug substances. 1-(4-Nitrophenyl) piperazine (4-NPP) was selected as a new derivatization reagent because it shifted well the benzyl halides derivatives away to the near visible range (392 nm), which could minimize the matrix interferences from the drug substances and related impurities. Meanwhile, potassium iodide (KI) was used to convert the mixed benzyl halides into benzyl iodides before derivatization. The derivatization parameters were also optimized using the design of experiments (DoE) for achieving the best reaction efficiency. The results showed that the new approach had high specificity and sensitivity, and the LOQs were 7–9 μg g−1 relative to 5 mg mL−1 antipyrine and 17.5–22.5 μg g−1 relative to 2 mg mL−1 oroxylin A. The method is a valuable alternative for the determination of residual benzyl halides in the drug substances.
研究领域:
药物分析
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毒理学
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产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2023
·Vol. 28
·期 14
·5309
·
IF 4.6
Shi-Hui Lu,Xiao-Na Liang,Xiao-Jin Nong,Ran Chen,Xiu-Xia Li
Trans-p-hydroxycinnamic acid and its esters in the leaves ofLigustrum robustummight be a new resource to prevent diabetes and its complications. In the present study, a new HPLC-UV method using hydrolyzation with sodium hydroxide for quantitation oftrans-p-hydroxycinnamic acid and totaltrans-p-hydroxycinnamic acid esters in the leaves ofL. robustumwas developed, since it was difficult and troublesome to analyze no less than 34trans-p-hydroxycinnamic acid esters by usual HPLC. The extract ofL. robustumwas hydrolyzed with sodium hydroxide at 80 °C for 2 h, and then, hydrochloride was added. HPLC analysis was performed in reverse phase mode using a C-18 column, eluting with methanol-0.1% acetic acid aqueous solution (40:60,v/v) in isocratic mode at a flow rate of 1.0 mL·min−1and detecting at 310 nm. The linear range fortrans-p-hydroxycinnamic acid was 11.0–352.0 μg·mL−1(r2= 1.000). The limit of detection and limit of quantification were 2.00 and 6.07 μg·mL−1, respectively. The relative standard deviations of intra-day and inter-day variabilities fortrans-p-hydroxycinnamic acid were less than 2%. The percentage recovery oftrans-p-hydroxycinnamic acid was 103.3% ± 1.1%. It is the first HPLC method using hydrolyzation for quantification of many carboxylic esters. Finally, the method was used successfully to determinetrans-p-hydroxycinnamic acid and totaltrans-p-hydroxycinnamic acid esters in various extracts of the leaves ofL. robustum. The 60–70% ethanol extracts ofL. robustumshowed the highest contents of freetrans-p-hydroxycinnamic acid (3.96–3.99 mg·g−1), and the 50–80% ethanol extracts ofL. robustumdisplayed the highest contents of totaltrans-p-hydroxycinnamic acid esters (202.6–210.6 mg·g−1). The method can be applied also to the quality control of the products ofL. robustum.Keywords:trans-p-hydroxycinnamic acid;esters;Ligustrum robustum;HPLC-UV;hydrolyzation;sodium hydroxide;quantification
研究领域:
植物化学
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分析化学
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药用植物研究
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Xinmiao Wang,Qian Wang,Dong Cai,Jinghan Yu,Xuan Chen,Xu Guo,Peiyong Tong,Xiaoyang Liu,Fawen Yin,Dayong Zhou
HPLC-UV analysis was used to evaluate the enzymatic degradation characteristics of tyrosol acyl esters (TYr-Es) and alkyl gallates (A-GAs). Among various hydrolytic enzymes, TYr-Es can be hydrolyzed by pancrelipase, while A-GAs cannot be hydrolyzed by pancrelipase. Interestingly, carboxylesterase-1b (CES-1b), carboxylesterase-1c (CES-1c) and carboxylesterase-2 (CES-2) are able to hydrolyze TYr-Es and A-GAs, and thus to liberate tyrosol (TYr) and gallic acid (GA). By contrast, the degrees of hydrolysis (DHs) of TYr-Es and A-GAs by CES-1b and CES-1c were significantly higher than those by CES-2. Meanwhile, the DHs of TYr-Es were much higher than those of A-GAs. Especially, the DHs firstly increased and then decreased with the increasing alkyl chain length. Besides, DHs positively correlated with the unsaturation degree at the same chain length. Through regulating carbon length, unsaturation degree and the ester bond structure, controlled-release of phenolic compounds and fatty acids (or fatty alcohols) from phenolic esters will be easily achieved.
研究领域:
生物化学
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食品科学
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产品关联
DOI
PubMed
高影响因子
INDUSTRIAL CROPS AND PRODUCTS
·
2024
·
IF 5.6
Weikang Shen,Haobo Wang,Zhouzhe Lan,Guangzhi Xu,Qinxue Ni,Qiufen Mo,Youzuo Zhang,Yan Wang
Gardenia fruit oil (GFO) is a new emerging edible woody oil with few investigations of its’ refinement process. In this study, different degumming, deacidification and bleaching technologies were introduced for realizing moderate refining of the GFO based on the preservation of bioactive micronutrients. Firstly, a simple multi-stage solid phase extraction (SPE) combined with a lab- affordable HPLC-UV instrument was developed for determinations of several vital biological constituents, such as crocetin, geniposide, polyphenols, phytosterols and squalene in the GFO. Satisfactory limit of detection (LOD), limit of quantification (LOQ), recovery, intra-day and inter-day precision were obtained. Subsequently, changes of those phytochemicals during three types of degumming, followed by three kinds of deacidification and then three ways of bleaching were investigated, offering insightful suggestions for achieving moderate refining of the GFO. Finally, the refined GFO might be suggested as a potential functional edible oil with valuable micronutrients. To our knowledge, this is the first study investigating moderate refinement techniques for GFO, as well as developing novel methods for phytonutrients analysis in the GFO.
研究领域:
食品科学
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分析化学
·
植物化学
✓ 已验证
产品关联
DOI
高影响因子
Analytical Methods
·
2018
·Vol. 10
·期 11
·1325-1330
·
IF 2.073
Yong Zhang,Zhizhong Zou,Guixing Chou
To quickly determine the amounts of kirenol, darutoside and darutigenol in Herba Siegesbeckiae using HPLC, the efficiency of sample cleanup with different solid phase extraction methods was systematically investigated. The results showed that a polymer based strong anion exchange (P-SAX, 200 mg/6 mL) sorbent could separate and enrich diterpenoids providing rapid determination without impurity interference. In this paper a new HPLC-UV method using a core–shell column (Boltimate C18 3.0 × 100 mm, 2.7 μm) for the quantitative determination of three diterpenoids was developed. Under optimum experimental conditions, P-SAX pretreatment with a core–shell analytical column exhibited satisfactory results in the determination of diterpenoids in Herba Siegesbeckiae with recovery rates of 95–102%, relative standard deviations below 1.1%, a limit of quantitation as low as 0.1 6 μg mL−1, and a short analytical runtime of 8 min. Finally, the proposed method was successfully applied in the profiling of diterpenoids in Herba Siegesbeckiae from different regions.
研究领域:
分析化学
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生药学
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植物科学
✓ 已验证
产品关联
DOI
高影响因子
Drug Research
·
2023
·Vol. 73
·期 06
·335-340
·
IF 2.2
Guo Haihua,Zhang Rui,Deng Liangjun,Li Meng,Li Sha,Zhao Suqing
Background Inhalation preparation involves liquid or solid raw materials for delivering to lungs as aerosol or vapor. The liquid preparation for nebulizer is effective for convenient use and patient compliance and it has been extensively used in the treatment of clinical lung diseases. Clinical staff often mixes the compound ipratropium bromide with beclomethasone propionate and budesonide inhaler but reference values of inhalants for clinical use need to be established for simplifying the operation procedure. The high-performance liquid chromatography (HPLC) method of compound ipratropium bromide solution, beclomethasone propionate suspension and budesonide suspension after mixed atomization was studied. Methods The specificity, linearity, recovery (accuracy), precision and stability of compound ipratropium bromide, beclomethasone propionate and budesonide were tested to verify the developed liquid phase method. Results The developed liquid phase method had high specificity, linear R2≥0,999, recovery (accuracy) RSD (relative standard deviation) less than 2%, precision RSD less than 2,0%, and stability RSD less than 2,0%. Conclusion The liquid phase methodology developed in this study can be used for the determination of compound ipratropium bromide mixed with beclomethasone propionate and budesonide. The current methodology can also be used to provide a reference for the determination of its content after mixing, and further data support for its clinical medication.
研究领域:
药物分析
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色谱学
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药学
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临床药理学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2023
·
IF 8.8
Li Gao,Piao Xu,Jiaoyan Ren
This work described a sensitive and economical HPLC-UV method with FDAA derivatization to simultaneously detect 36 D/ l -amino acids, which provides higher sensitivity and lower cost than other HPLC-based methods. It was validated for linearity range (8–1000 µmol/L), limits of detection (2.68–62.44 pmol/L), limits of quantification (2.93 to 208.13 pmol/L), intraday precision (0.30 % − 5.31 %), interday precision (1.96 % − 8.04 %) and accuracy (86.53 % − 121.46 %). This method was then applied in the determination of D/L- amino acids abundance in fermented and unfermented food materials and showed the characteristics of each type of foods. The method also demonstrated good performance in another application case for the discrimination of different types of food materials based on D/L- amino acids profile. It emphasizes the ability of the method to study the characteristics, distribution and abundance of d -amino acids in foods and their potential application in food quality control.
研究领域:
分析化学
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食品科学
·
生物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Heliyon
·
2023
·
IF 4
Hengyi Yu,Dongyan Li,Dong Xiang,Xiping Li,Lu Liu,Dong Liu,Xuepeng Gong
A rapid, specific and accurate high-performance liquid chromatography with tunable ultraviolet detection method was developed to simultaneously determine azathioprine metabolites, 6-thioguanine nucleotides (6-TGN) and 6-methyl mercaptopurine riboside (6-MMPr) in human red blood cells. Erythrocyte lysate sample was precipitated by perchloric acid under the protection of dithiothreitol, with 6-TGN and 6-MMPr being acid hydrolyzed to produce 6-thioguanine (6-TG) and 6-methymercaptopurine (6-MMP). A Waters Cortecs C 18 column (2.1 × 150 mm, 2.7 μm) was used for chromatographic separation with a water (containing 0.01 mol/L ammonium acetate and 0.2% acetic acid)/methanol linear gradient at a flow rate of 0.45 mL/min in a 5.5 min. UV detection wavelengths were 340 nm for 6-TG, 303 nm for 6-MMP and the IS (5-bromouracil). The calibration curves fitted a least squares model (weighed 1/ x 2 ) from 0.15 to 15 μmol/L for 6-TG ( r 2 = 0.9999) and from 1 to 100 μmol/L for 6-MMP ( r 2 = 0.9998). This method was validated according to the FDA bioanalytical method validation guidance and ICH M10 bioanalytical method validation and study sample analysis guidance for industry, and successfully utilized in ten IBD patients receiving azathioprine therapy.
研究领域:
药理学
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分析化学
·
临床化学
✓ 已验证
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）