PHYTOCHEMICAL ANALYSIS
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2022
·Vol. 33
·期 8
·1246-1256
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IF 3.024
Ying Xu,Yiqun Wan,Fan Liu,Jinping Chen,Ting Tan,Lan Guo
Introduction Anthraquinones are considered to be an important class of bioactive substances in Cassiae semen , and the content of anthraquinones is an essential indicator of the quality of Cassiae semen raw herbal materials. Objectives The present study aimed to propose a novel, efficient and effective ultra-high-performance liquid chromatography (UHPLC) method for the simultaneous determination of aurantio-obtusin, aloe-emodin, rhein, obtusin, emodin, chrysophanol and physcion, with the help of natural deep eutectic solvents (NADESs) as extraction solvents. Methodology NADESs were introduced to the simultaneous extraction of anthraquinones from Cassiae semen samples. Several NADESs were designed by menthol, choline chloride, d -glucose as hydrogen bond acceptors, with nine different acids and appropriate water as hydrogen bond donors. The parameters affecting the extraction efficiency of seven anthraquinones were demonstrated in detail. Results Among the obtained NADESs, the highest extraction efficiency was demonstrated by a solution consisting of d -glucose, lactic acid and water with a molar ratio of 1:5:4. The seven anthraquinones were separated on an ACQUITY UPLC® BEH C 18 column (2.1 mm × 100 mm, 1.8 μm) and detected within 12 min by a photodiode array (PDA) detector at 254 and 284 nm. The limits of detection and quantitation were from 1.00 to 7.26 μg/l and 3.29 to 24.22 μg/l, respectively. And Cassiae semen sample-based recoveries ranged from 81.13% to 113.78% with the relative standard deviation (RSD) ( n = 6) of 1.4% to 10.1%. Conclusion The developed method demonstrated that NADESs were applied successfully to analyse the anthraquinones in Cassiae semen samples collected from different regions in China.
研究领域:
中药学
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分析化学
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DOI
高影响因子
CHROMATOGRAPHIA
·
2024
·
IF 1.2
Han Kyoung-Moon,Woo In Suk,Park Chae Gyeong,Kim You Kyung,Yang Yoon Ji,Park Bo Reum,Choi Jang Duck,Son Kyung Hun
Preservatives can be used in natural and organic cosmetics to prevent quality deterioration during distribution and use, but the ingredients permitted are limited in the Republic of Korea. A method of simultaneous analysis was developed to monitor natural and organic cosmetics distributed online for the presence of 15 illegally used preservatives. Considering the complexities of the cosmetic matrices, an optimized sample preparation method is essential. Therefore, we developed the optimal purification method by comparing three preparation methods: QuEChERS, high-speed centrifugation, and solid-phase extraction (SPE). The SPE method, which exhibited the most favorable results in matrix reduction, was employed. To establish the SPE-ultra-high-performance liquid chromatography-diode array detection method, factors such as the mobile phase and column were optimized. The optimal separation of the 15 preservatives was observed under the following conditions: mobile phase A comprising 0.1% phosphoric acid in water with 0.5 mM sodium hexanesulfonate and a C 8 column (1.7 μm, 2.1 × 150 mm) as the stationary phase. The linear correlation coefficients were > 0.9998, and the limits of detection and quantitation ranged from 0.05 to 0.67 and 0.15 to 2.02 μg mL −1 , respectively. Using the established analytical method, illegally used preservatives were detected in products claimed to be natural and organic cosmetics sold on the market, and these findings were subsequently verified using liquid chromatography-tandem mass spectrometry. Six out of 47 samples contained phenoxyethanol and parabens. Therefore, this method will help manage the addition of illegal preservatives to natural and organic cosmetics.
研究领域:
分析化学
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化妆品科学
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产品关联
DOI
高影响因子
Foods
·
2022
·Vol. 11
·期 3
·386
·
IF 5.561
Ying Xu,Xuan Yu,Jiaqi Gui,Yiqun Wan,Jinping Chen,Ting Tan,Fan Liu,Lan Guo
A rapid and effective ultra-high performance liquid chromatography (UHPLC) method was developed for the determination of five anthraquinones (emodin, physcion, aloe-emodin, rhein, and chrysophanol) inPolygonum multiflorum. The target compounds were ultrasonically extracted with 70% methanol, followed by dispersive solid-phase extraction (d-SPE) with HC-C18 and desorption with acetonitrile. The five anthraquinones were separated on an ACQUITY UPLC®HSS T3 column (2.1 × 100 mm, 1.8 μm) and detected by a photodiode array detector (PDA) at 254 nm. Under the optimized conditions, linear relationships were achieved in the range of 0.3~100 mg/L for emodin, 0.3~40 mg/L for physcion, 0.1~20 mg/L for aloe-emodin, and 0.05~20 mg/L for rhein and chrysophanol. The limits of detection of the five analytes ranged from 0.01 to 0.08 mg/L, and the recoveries were within the range of 82.8~118.4% with an RSD (n= 6) of 1.0~10.3%. The intra-day and inter-day precision (n= 5) of the five targets were in the range of 1.0~1.8% and 3.0~3.1%, respectively. Furthermore, this method was applied to analyses ofPolygonum multiflorumsamples collected from different regions in China with satisfactory results. All the results indicated that this method is suitable for the detection of five anthraquinones inPolygonum multiflorum.Keywords:anthraquinones;Polygonum multiflorum;d-SPE;UHPLC
研究领域:
分析化学
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中药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
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2013
·
IF 0.565
Erqun Song,Li Xu
In the present study, a method based on ultra-fast liquid chromatography (UFLC) was successfully developed for chromatographic fingerprint (CFP) analysis of Glycyrrhizae radix. The CFP analysis was performed on an Agilent ZorBax XDB-C18 column (2.1 × 100 mm, 1.8 µm) using a gradient elution of methanol and water (containing 1% acetic acid) within a runtime of 30 min. The method was validated by eleven common peaks that were shown in all samples. The results revealed that the method was precise, stable, and reproducible. Using the established method, three Glycyrrhizae radix samples from different sources were evaluated for their similarity. Compared to the conventional high performance liquid chromatography, UFLC provided many advantages, such as time saving, less solvent consumption and better separation efficiency. It was a reliable and powerful method for quality control of traditional Chinese medicines with multi-components.
研究领域:
中药学
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分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
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2015
·Vol. 38
·期 6
·886-893
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IF 2.737
Juanjuan Pi,Xia Wu,Shitian Yang,Pingyan Zeng,Yifan Feng
A rapid, sensitive, and reliable approach for analyzing five kinds of erythrocyte phospholipids in Sprague–Dawley rats was provided by ultra high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry with MassLynx TM MassFragment. Improving conventional high performance liquid chromatography techniques, ultra high performance liquid chromatography integrated with quadrupole time-of-flight tandem mass spectrometry offers high sensitivity and increased analytical speed by using columns packed with sub-2 μm particles (1.7 μm), which allows a faster separation to be achieved. Through this method, 83 phospholipids were tentatively characterized based on their mass spectra and tandem mass spectra, as well as by matching the in-house formula database within a mass error of 5 ppm, including 40 phosphatidylcholines, 24 phosphatidyl ethanolamines, three phosphatidylinositols, six phosphatidylserines, and ten sphingomyelins. Our present results proved that the established method could be used to qualitatively analyze complex erythrocyte phospholipids in Sprague–Dawley rats and provide a useful data base for pharmacology and phospholipidomics to seek potential biomarkers of disease prediction.
研究领域:
分析化学
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生物化学
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医学
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产品关联
DOI
PubMed
高影响因子
Food Analytical Methods
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2020
·Vol. 13
·期 8
·1666-1672
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IF 2.667
Gao Yuling,Li WeiQing,Li Dongxue,Yan Rui,Guo Yongxia
A novel procedure was developed for the determination of DCPTA residues in mung bean using dispersive solid-phase extraction (DSPE) couple with ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). Sample was extracted with a HAc-acetonitrile solution (1:99, V/V) and primarily purified by DSPE with C 18 , PSA, and GCB as absorbent. In order to detect DCPTA residues from mung bean, retention time, quantitative ions, and qualitative ions were used for screening and confirmation. The effect DSPE conditions of the type and dosage of adsorbents and extraction condition were researched, and then the suitable method was founded. Under the optimized conditions, the detection limit (S/N = 3) and quantitative limit (S/N = 10) of DCPTA were 0.11 μg kg −1 and 0.37 μg kg −1 , respectively. The average recoveries ranged from 93.8 to 96.8% at spiking levels of 1.0, 5.0, and 10.0 μg kg −1 , with a relative standard deviation (RSD) lower than 6.2% ( N = 6). This method is simple, accurate, and sensitive, and is suitable for the rapid screening and confirmatory analysis of plant growth regulator residues in coarse grains.
Graphical abstract
研究领域:
分析化学
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食品科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2024
·
IF 2.8
Feng Xu,Jiayong Yu,Yinliang Wu
An integrated method combining solid-phase extraction (SPE) with ultra-performance liquid tandem mass spectrometry (UPLC-MS/MS) has been established for quantifying bacitracin (BTC), bacitracin zinc (BZ), and bacitracin methylene disalicylate (BMD) in animal feed. A pretreatment procedure that can effectively, quickly, and simultaneously extract and purify BTC, BZ, or BMD in feed was developed for the first time through the optimization of extraction and SPE conditions. After extraction with acetonitrile + methanol + 15 % ammonia solution (1:1:1, v : v : v ) and dilution with EDTA solution (1.5 mmol/L, pH 7.0), a SPE procedure was carried out with C 18 cartridge. Following LC-MS/MS analysis utilized a Waters Peptide BEH C 18 column with a gradient elution of 0.1 % formic acid in water/acetonitrile with. This method demonstrated a strong linear correlation (R 2 > 0.9980) across a 0.01–1.0 mg/L concentration span, based on a matrix-matched standard curve. Satisfactory recoveries of BTC (bacitracin A, B 1 , B 2 , and B 3 ), BZ, and BMD in different feeds were obtained from 80.7 % to 108.4 %, with relative standard deviations below 15.7 %. Low limits of quantification ranging within 7.2–20 μg/kg were achieved for bacitracin A , B 1 , B 2 , and B 3 . This method provided an effective and reliable detection method to prevent the addition of BTC and different BTC formulations in feeds.
研究领域:
分析化学
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兽医学
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食品安全
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产品关联
DOI
PubMed
高影响因子
INDUSTRIAL CROPS AND PRODUCTS
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2019
·
IF 4.191
Yu-Han Hu,Qiu-Yan Wang,Li-Hong Ye,Juan Yang,Xin Dong,Hui Zheng,Jian Zhou,Jun Cao
A simple, rapid and environmentally friendly method named effervescence-assisted matrix solid-phase dispersion (EA-MSPD) was investigated for the extraction of four coumarins (esculin, esculetin, fraxin and fraxetin) from Crotex fraxini ( C. fraxini ). In this study, an effervescent tablet containing carbon dioxide sources (100 mg sodium bicarbonate and 200 mg sodium dihydrogenphosphate) and an adsorbent (25 mg benzo-15-crown-5) was prepared. The effervescent tablet was dissolved into an aqueous solution, and as a consequence of the effervescence reaction, carbon dioxide was generated, thus making the sample better a dispersion of the extraction solvent (100 mM sodium dodecyl sulfate). The variables that influenced the extraction efficiency included effervescent salts, extraction solvents and crown ether. These values were represented using ultra- high-performance liquid chromatography (UHPLC). Good linearity was exhibited by coefficients of determination all equal to 1, limits of detection ranging from 1.62 to 3.83 ng·mL −1 and limits of quantification ranging from 5.39 to 12.76 ng·mL −1 . The recoveries ranged from 91.37 to 100.29% with relative standard deviations of 0.57–4.58% under optimized conditions. In this work, the proposed EA-MSPD method was successfully applied to extract and identify four coumarins in C. fraxini . Compared with previously reported methods, the method examined herein was faster, greener and more sensitive.
研究领域:
分析化学
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药学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF ETHNOPHARMACOLOGY
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2013
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IF 2.755
Yan Lou,Jinqi Zheng,Baohong Wang,Xingguo Zhang,Xia Zhang,Su Zeng
Ethnopharmacological relevance Stellera chamaejasme L. (Thymelaeaceae) was a toxic perennial herb and widely used as pesticide and dermatological agents in China. Chamaechromone was a major component in the dried roots of Stellera chamaejasme with anti-HBV and insecticidal activity. Analysis of metabolic profile in vivo and in vitro plays a pivotal role to unravel how TCM works. And the metabolites of chamaechromone might influence the effects and toxicity of Stellera chamaejasme . Moreover, the metabolic routes of chamaechromone provide an important basis for toxicological safety evaluation. Until now, little is known about the metabolism of chamaechromone. The current study was designed to characterize the whole metabolic pathways of chamaechromone in vitro and in vivo . Materials and methods Twenty-four rats were randomly divided into four groups, including two oral administration groups (100 mg kg −1 ), one intravenous injection group (5 mg kg −1 ), and one control group. The metabolites in rat urine and feces and bile were identified by UPLC/Q-TOF MS analysis and β-glucuronidase hydrolysis. Moreover, the possible metabolic mechanism was further confirmed by Phase I and Phase II metabolism and catechol- O -methyltransferase methylation in rat liver S9 fraction and degradation in rat intestinal bacteria . Results A total of 24 metabolites from chamaechromone were detected and identified in vivo and in vitro , 20 of which were novel. And the major metabolic processes were hydroxylation, methylation, glucuronation, acetylation, dehydroxylation and degradation. Conclusions The present study revealed the whole metabolic pathways of chamaechromone in rat through both in vitro and in vivo experiments for the first time. And chamaechromone could undergo extensive phase I and phase II metabolism in rat. These findings would provide an important basis for the further study and clinical application of chamaechromone. In addition, the results of this work have showed the feasibility of the UPLC/Q-TOF-MS approach for rapid and reliable characterization of metabolites.
研究领域:
民族药理学
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药物代谢
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毒理学
✓ 已验证
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2017
·
IF 4.529
Fenglian Wang,Minyi Cao,Nani Wang,Nadeem Muhammad,Shuchao Wu,Yan Zhu
Folic acid plays a significant role during periods of rapid cells division and growth. Pregnant women require folic acid daily, either from dietary supplements or folic acid tablets in order to prevent fetal neural tube defects. In this work, a simple coupled ultrahigh performance liquid chromatography and ion chromatography technique was developed for simultaneous determination of folic acid and inorganic anions in folic acid tablets. A reversed-phase C18 column was used as the pretreatment column for on-line separating inorganic anions from organics. Inorganic anions were concentrated in the concentration column. Under the optimal chromatographic conditions, good sensitivity and linear calibration-curves (r ≥ 0.9992) were obtained. Low detection limits were obtained in the range of 0.0032–0.40 mg L −1 for all analytes. Repeatability results were satisfactory with relative standard deviations less than 1.50% (n = 5). The developed method was utilized to analyze spiked folic acid tablet samples with good measured recoveries (92.4–107.4%).
研究领域:
分析化学
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医学
·
药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Jove-Journal of Visualized Experiments
·
2018
·
IF 1.184
Ya-Min Du,Shen-Li Zheng,Li Liu,Josef Voglmeir,Gabriel Yedid
In recent years, the carbohydrate moieties of plants have received considerable attention, as they are a potential source of cross-reactive, allergy-provoking immune responses. In addition, carbohydrate structures also play a critical role in plant metabolism. Here, we present a simple and rapid method for preparing and analyzing N-glycans from different cultivars of radish (Raphanus sativus) using an N-glycanase specific for the release of plant-derived carbohydrate structures. To achieve this, crude trichloroacetic acid precipitates of radish homogenates were treated with PNGase H+, and labeled using 2-aminobenzamide as a fluorescent tag. The labeled N-glycan samples were subsequently analyzed by ultra performance liquid chromatography (UPLC) separation and matrix-assisted laser desorption ionization-time of flight (MALDI-TOF) mass spectrometry for a detailed structural evaluation and to quantify relative abundancies of the radish-derived N-glycan structures. This protocol can also be used for the analysis of N-glycans from various other plant species, and may be useful for further investigation of the function and effects of N-glycans on human health.
研究领域:
植物学
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分子生物学
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免疫学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
PHYTOMEDICINE
·
2016
·
IF 2.937
Hao Sun,Guangwen Luo,Zheng Xiang,Xiaojun Cai,Dahui Chen
Background The selection of effect indicators in the pharmacokinetic/ pharmacodynamic study of complex diseases to describe the relationship between plasma concentration and effect indicators is difficult. Purpose Three effect indicators of renal fibrosis were successfully determined. The relationship between pharmacokinetics and pharmacodynamics of rhein in rhubarb was elucidated. Study design The study was a metabolomics analysis of rat plasma and pharmacokinetics/ pharmacodynamics of rhein. Methods A sensitive and simple ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-MS/MS) method was applied to determine the rhein plasma concentration in the rat model of renal fibrosis and rat sham-operated group after the administration of rhubarb decoction . Then, the ultra performance liquid chromatography-Micromass quadrupole-time of flight mass spectrometry (UPLC-QTOF/MS) metabolomics method was used to screen biomarkers of renal fibrosis in rat plasma. Furthermore, the relationship between the plasma concentration of rhein and the concentration of three biomarkers directly related to renal fibrosis were analyzed. Results The three screened biomarkers could represent the effect of rhein treatment on renal fibrosis. Increasing the plasma concentration of rhein tended to restore the concentration of the three biomarkers in the model group compared with that in the sham-operated group. Evident differences in the area under the plasma concentration-time curve (AUC) of rhein were also observed under different pathological states. The results provide valuable information for the clinical application of rhubarb. Conclusion Rhein intervention could recover the physiological balance in living organisms from the pharmacokinetic/pharmacodynamic levels. New information on the pharmacokinetic/pharmacodynamic study of complex diseases is provided.
研究领域:
药理学
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肾病学
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代谢组学
✓ 已验证
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）