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
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产品关联
DOI
PubMed
Analytical Methods
·
2017
·Vol. 9
·期 22
·3361-3374
·
IF 1.9
Zhi Liu,Hai-Long Wu,Li-Xia Xie,Yong Hu,Huan Fang,Xiao-Dong Sun,Tong Wang,Rong Xiao,Ru-Qin Yu
In the present work, a novel chemometrics-assisted analytical strategy that combines three-way high performance liquid chromatography-diode array detection (HPLC-DAD) data with a second-order calibration method based on the alternating trilinear decomposition (ATLD) algorithm was developed for direct, accurate and simultaneous determination of thirteen phenolic compounds in complex red wine samples without an intricate clean-up step. All analytes were rapidly eluted out (7.5 min) under a simple gradient LC-separation and then detected in a multi-channel UV window. With the aid of the prominent “second-order advantage” of the ATLD algorithm, four common HPLC problems, i.e. solvent peaks, peak overlaps, unknown interferents and baseline drifts, could be mathematically calibrated, enabling “pure signals” of analytes to be extracted out from interference-heavy but information-rich HPLC-DAD profiles. The new strategy could avoid the loss of analytes of interest to significantly improve the analytical accuracy. Validation parameters, i.e. recovery (97.7–104%), precision (RSD < 7.1%), matrix effect, limits of detection (LODs, 0.02–0.27 μg mL−1) and limits of quantitation (LOQs, 0.06–0.82 μg mL−1) of thirteen analytes, were surveyed and further confirmed by the LC-MS/MS method. Based on the indexes of phenolic compositions in wines, pattern recognition methods, i.e. principal component analysis and linear discriminant analysis (PCA-LDA), were applied for distinguishing wines of different storage years, and the discriminant accuracies were higher than 90%, which proved that this chemometrics-assisted HPLC-DAD strategy was an excellent method for direct and accurate determination of phenolic compositions in complex wine samples as well as the authentication of vintage year.
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
Chinese Journal of Natural Medicines
·
2012
·
IF 0
Yi LI,Ming RUAN,Jian-Guang LUO,Ling-Yi KONG
A novel on-line method using high performance liquid chromatography (HPLC) with a diode array detector (DAD) and a chemiluminescence (CL) detector was successfully developed for simultaneously analyzing the antioxidant efficacies of 15 components in Guan-Xin-Ning (GXN) injection, a traditional Chinese medicinal preparation consisting of Radix Salvia miltiorrhiza and Rhizoma Ligusticum chuanxiong for the treatment of coronary heart disease and angina pectoris. The analytical conditions were optimized, validated and applied to determine H 2 O 2 inhibition rates of the 15 phenolic acids in GXN injections from 14 different production batches. The results showed that antioxidant diversities were found in the 15 compounds and that danshensu, protocatechuic aldehyde and rosmarinic acid were largely responsible for the antioxidant activity of GXN injection (25.82%-51.19%). In addition, 14 batches of GXN injections were divided into five groups corresponding with five different factories by principal component analysis (PCA) assay. Therefore, the proposed HPLC-DAD-CL method was simple, rapid and low-cost for screening antioxidant constituents in a complex system, which can be used to reveal the antioxidant mechanism of GXN injection and is applicable for its quality control in terms of activity, which was different from the routine chemical assessment.
研究领域:
中药学
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分析化学
✓ 已验证
产品关联
DOI
Evidence-based Complementary and Alternative Medicine
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2023
·
IF 2.65
Wei-Qi Yang,Zheng-Ming Qian,Meng-Qi Wu,Jian-Li Gao,Qi Huang,Yuan-Sheng Zou,Dan Tang
The root of Polygonum bistorta (PB) is a traditional Chinese medicinal plant material widely used in China. It has been commonly used for the treatment of hemostasis, detumescence, diarrhea, snake bite, and acute gastroenteritis. However, the research on the antioxidant properties and bioactive compounds from PB is inadequate. In the current research, an online microextraction (OLME) coupled with a high-performance liquid chromatography coupled with the 2,2-nitrogen-di (3-ethyl-benzothiazole-6-sulfonic acid) diammonium salt antioxidant assay (HPLC-ABTS) system for rapid analysis of antioxidants from PB was proposed. The PB sample (0.17 mg) was online extracted by mobile phase (acetonitrile and 0.2% acetic acid); a Poroshell 120 SB-Aq column was used for separation; then, an online ABTS assay system was used for screening the antioxidants. Finally, ten components were found in PB, and among them, eight components possessed antioxidant activities. Furthermore, five components (gallic acid, neochlorogenic acid, caffeic acid, chlorogenic acid, and an unknown compound) were proved as major antioxidants when compared with rutin as an antioxidant marker. The results showed that the developed OLME-HPLC-ABTS system was a simple, rapid, green, and efficient instrument for the screening of antioxidants from PB, which provides a powerful tool for the discovery of natural antioxidants in Chinese medicines.
研究领域:
生药学
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分析化学
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天然产物
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中医药
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2022
·Vol. 36
·期 10
·e5435
·
IF 1.911
Jing Zhang,Jun-qing Yang,Ying Luo,Jian-sha Li,Tao Gong,Su-qiong Huang,Yan Xiong,Xin-hui Jiang
The study of brain diseases has long been of interest to researchers worldwide, and stroke is the third leading cause of death that threatens human health. At the same time, cerebral ischemia–reperfusion injury is closely associated with high rates of disability and mortality. The conditions of the 6-aminoquinolyl N -hydroxysccinimidyl carbamate method for the derivatization of amino acids in the bone marrow fluid and hippocampus of C57BL/6 mice with cerebral ischemia–reperfusion injury were explored and optimized, such as the column temperature, concentration of derivatization reagents and mobile phase concentration. The mobile phase consisted of 20 m m sodium acetate solution (phosphoric acid to adjust pH 5.0) and 60% acetonitrile solution at a flow rate of 1 ml min −1 . The 23 analytes were separated and determined in a gradient elution procedure; the correlation coefficient r was >0.9990 in the range 0.1–8.0 μg ml −1 . The results showed that the content of relevant analytes was significantly changed in the cerebral ischemia–reperfusion injury model, and the method was suitable for the simultaneous determination of 23 amino acids in the bone marrow fluid and hippocampus of C57BL/6 mice.
研究领域:
神经生物学
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分析化学
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产品关联
DOI
PubMed
高影响因子
CHROMATOGRAPHIA
·
2023
·Vol. 86
·期 8
·595-603
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IF 1.7
Huang Dan,Tian Yufei,Zheng Yili,Li Mengyu,Xu Xia,Chen Hongyuan,Rui Wen
Forced degradation studies aim to systemically characterize the degradation products of an active pharmaceutical ingredient (API) and its formulations under harsh conditions that accelerate degradation. These studies are especially valuable for sustained-release products in selecting appropriate packaging materials and storage conditions in the field of pharmaceutics. To demonstrate the degradation pathways and degradation products of the API and products, mass spectrometry is used for further characterization of the degradation products. Goserelin acetate sustained-release implant, which is prepared by hot melt extrusion using biodegradable material polylactic acid-glycolic acid copolymer as a carrier, is used for the treatment of early breast cancer in premenopausal and perimenopausal women. In this study, a simple and sensitive high-performance chromatography method was established following the ICH guidance. We conducted forced degradation experiments to determine the conditions of the product. The forced degradation studies of the goserelin acetate sustained-release implant showed the presence of a single impurity during thermal degradation, as observed in the HPLC analysis. To elucidate the structure of the impurity and characterize its degradation pathway, we performed further characterization using LC–MS.
研究领域:
药学
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分析化学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
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2021
·Vol. 44
·期 9
·1852-1865
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IF 3.645
Jingjing Wu,Song Zhang,Jiali Li,Xiaoli Zhong,Guiping Feng,Liangqing Hu,Fan He,Hanjing Cen,Yilu Chen,Yanling He,Huasong Zeng,Xiao Chen,Xiaolan Mo
Low-dose methotrexate is the first-line therapy for juvenile idiopathic arthritis. In vivo, methotrexate is converted into a series of methotrexate polyglutamates whose intracellular levels contribute significantly to its efficacy and toxicity. In this study, a novel high-performance liquid chromatography–tandem mass spectrometry method was developed and validated to simultaneously determine erythrocyte methotrexate polyglutamates using stable isotope-labeled internal standards. Erythrocyte samples were precipitated by perchloric acid and then determined on an XBridge BEH C18 column with an XP vanguard precolumn in 12 min. The mobile phase consisted of 10 nM ammonium acetate (pH 10) and methanol under gradient elution. The detection was carried out in multiple reaction monitoring mode via an electrospray ionization source in positive ionization mode. The calibration curve for each metabolite was linear from 2.0 to 500.0 nmol/L ( r 2 > 0.99). The intraday and interday accuracies were between 93.0 and 107.0%, and the corresponding precisions were between 0.8 and 5.2%. The relative recovery ranged from 82.7 to 105.1%, and the relative matrix effect varied from 96.5 to 104.4%. The erythrocyte metabolites were stable for 30 days at −80°C. This simple and accurate method is applicable to routine monitoring of the concentration of erythrocyte methotrexate polyglutamates in patients to achieve individualized treatment.
研究领域:
药理学
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分析化学
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临床医学
✓ 已验证
DOI
PubMed
高影响因子
ACS Omega
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2021
·
IF 3.512
Zhihui Lin,Yingnan Lin,Jianqi Lin,Yizhi Zhang,Song Fang
A modified QuEChERS method in combination with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was first developed for the determination of fenbutatin oxide in six types of samples (soil, tobacco, rice, milk, pork liver, and pork). Fenbutatin oxide was extracted with acetonitrile containing 1% formic acid (v/v) and purified by dispersive solid-phase extraction using primary secondary amine (PSA) and quantitatively analyzed by HPLC-MS/MS. In the range of 0.005–1 mg/kg, a good linear relationship exists between the concentration of fenbutatin oxide and the peak area, giving a coefficient of determination (R2) of >0.99. The recoveries of fenbutatin oxide at three spiked levels were 79.04–97.12% with the relative standard deviations (RSDs) of 3.30–10.96%, and the limit of quantification (LOQ) was 0.007 mg/kg. In addition, the developed method is consistent with the reference method (R2 = 0.9896, n = 40). The method is demonstrated to be convenient and reliable for the routine monitoring of fenbutatin oxide in soil and plant- and animal-derived foods.
研究领域:
分析化学
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食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Frontiers in Plant Science
·
2024
·
IF 4.1
Jiali Cheng,Fengxia Guo,Liyang Wang,Zhigang Li,Chunyan Zhou,Hongyan Wang,Wei Liang,Xiaofeng Jiang,Yuan Chen,Pengbin Dong
Introduction: The quality of traditional Chinese medicine is based on the content of their secondary metabolites, which vary with habitat adaptation and ecological factors. This study focuses on Lonicera japonica Flos (LJF), a key traditional herbal medicine, and aims to evaluate how ecological factors impact its quality.Methods: We developed a new evaluation method combining high-performance liquid chromatography (HPLC) fingerprinting technology and MaxEnt models to assess the effects of ecological factors on LJF quality. The MaxEnt model was used to predict suitable habitats for current and future scenarios, while HPLC was employed to analyze the contents of key compounds. We also used ArcGIS for spatial analysis to create a quality zoning map.Results: The analysis identified 21 common chromatographic peaks, with significant variations in the contents of Hyperoside, Rutin, Chlorogenic acid, Cynaroside, and Isochlorogenic acid A across different habitats. Key environmental variables influencing LJF distribution were identified, including temperature, precipitation, and elevation. The current suitable habitats primarily include regions south of the Yangtze River. Under future climate scenarios, suitable areas are expected to shift, with notable expansions in southern Gansu, southeastern Tibet, and southern Liaoning. The spatial distribution maps revealed that high-quality LJF is predominantly found in central and southern Hebei, northern Henan, central Shandong, central Sichuan, southern Guangdong, and Taiwan.Discussion: The study indicates that suitable growth areas can promote the accumulation of certain secondary metabolites in plants, as the accumulation of these metabolites varies. The results underscore the necessity of optimizing quality based on cultivation practices. The integration of HPLC fingerprinting technology and the MaxEnt model provides valuable insights for the conservation and cultivation of herbal resources, offering a new perspective on evaluating the impact of ecological factors on the quality of traditional Chinese medicines.
研究领域:
中药学
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生态学
✓ 已验证
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2024
·
IF 3.8
Wu Jiaxin,Yao Shunying,Wang Yiwei,Fan Sai,Cui Xia,Chen Dawei,Shi Zhixiong
Organophosphate esters (OPEs) are commonly used chemicals and are also regarded as emerging environmental pollutants. Recently, it has been proved that metabolites of OPEs (mOPEs) could also cause health concerns. However, analytical methods for the concurrent measurement of OPEs and mOPEs in human matrices are still complicated. In this study, a convenient and efficient analytical method combining a cold-induced strategy and HPLC–MS/MS was developed to simultaneously determine 18 OPEs and 10 mOPEs in human serum, urine, and human milk. In brief, after the sample was extracted with acetonitrile, a “one-step” treatment combining purification and enrichment was accomplished by cold-induced liquid–liquid extraction (CI-LLE), and analytes were then quantified by HPLC–ESI–MS/MS. The ratio of acetonitrile/water, and the temperature and time set in the CI-LLE procedure were optimized for achieving the highest enrichment factors. Under the best conditions, linearity, limits of detection (LODs), recovery, precision, and matrix effects of OPEs/mOPEs were verified. LODs of OPEs/mOPEs in serum, urine, and human milk were 0.1–113 pg/mL, 0.1–22 pg/mL, and 0.2–22 pg/mL, respectively. Average recoveries ranged from 80 to 123%, with relative standard deviations lower than 15% for most analytes. The matrix effect test showed slight signal enhancement or inhibition, and the use of isotopically labeled internal standards (ISs) could compensate for the effects. In real sample analysis, both OPEs and mOPEs showed high detecting frequency, which indicated their ubiquity in humans.
研究领域:
环境科学
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分析化学
·
毒理学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 4
·e70000
·
IF 1.7
Shuyan Xue,Feichao Song,Na Wei,Yuxuan Liu,Muchun Liu,Xi Huang,Yumeng Zhang,Yang Liu,Huiqin Hao,Junfeng Zhang
We aim to establish the fingerprint profile of Er Miao San (EMS) that aims to accurately evaluate the quality of EMS samples and to identify quality markers for different batches of EMS and explore its related targets and pathways for the treatment of rheumatoid arthritis. HPLC was employed with an Agilent C18 column. Cluster analysis and principal component analysis were conducted by using SPSS and SIMCA software. Network pharmacology techniques were utilized to explore the potential targets and pathways of EMS in the treatment of rheumatoid arthritis. The HPLC fingerprint profile of EMS was established, featuring a total of 15 common peaks, among which nine were identified. The 10 batches of medicinal materials could be clustered into three categories. With VIP > 1 as the criterion, four index differential components were screened out. These intersections were imported into the STRING database and Cytoscape software, resulting in 228 intersection targets. GO and KEGG enrichment analyses were performed on the related targets and pathways. The established method can effectively analyze the quality differences of EMS from different origins. The screened targets and pathways are of great significance for analyzing the differences in the treatment of rheumatoid arthritis by different batches of EMS.
研究领域:
中药学
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分析化学
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网络药理学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2014
·
IF 2.829
Guo Ma,Jiayuan Lin,Weimin Cai,Bo Tan,Xiaoqiang Xiang,Ying Zhang,Peng Zhang
Bilirubin, an important endogenous substances and liver function index in humans, is primarily eliminated via UGT1A1-catalyzed glucuronidation. Instability of bilirubin and its glucuronides brings substantial technical challenges to conduct in vitro bilirubin glucuronidation assay. In the present study, we developed a simple and robust HPLC method for simultaneous determination of unconjugated bilirubin (UCB) and its multiple glucuronides, i.e. bilirubin monoglucuronides (BMGs, including BMG1 and BMG2 isomers) and diglucuronide (BDG) in rat liver microsomes (RLM), human liver microsomes (HLM) and recombinant human UGT1A1 enzyme (UGT1A1) incubation systems, and applied it to study in vitro bilirubin glucuronidation. UCB, BMG1, BMG2, BDG and their isomers in the incubation mixtures were successfully separated using a C18 column with UV detection at 450 nm and mobile phase consisted of 0.1% formic acid in water and acetonitrile by a linear gradient elution program. Assay linearities of bilirubin were confirmed in the range 0.01–2 μM. Precision of UCB, BMG1, BMG2 and BDG ( n = 5) at low, medium and high concentration was within the range of RSD 0.4–3.7%, accuracy expressed in the mean assay recoveries of them ( n = 5) ranged from 92.8 ± 1.5% to 104.3 ± 2.2% for intra- and inter-day assays and the mean extraction recoveries of them ( n = 5) were above 91.5 ± 1.0%. Stability of bilirubin and its glucuronides was satisfactory at 37 °C in the incubation solutions during the reaction (30 min), 25 °C for 24 h and −70 °C for 7 d in the processed incubation samples with methanol. Furthermore, we established stable, reliable in vitro incubation systems and optimized the incubation conditions to characterize the kinetics of bilirubin glucuronidation by RLM, HLM and UGT1A1, respectively. The kinetic parameters of formation of total bilirubin glucuronides (TBG, the sum of BMG1, BMG2 and BDG) were as follows: K m of 0.45 ± 0.016, 0.40 ± 0.022, 0.44 ± 0.018 μM, V max of 2.65 ± 0.057, 1.86 ± 0.029, 2.95 ± 0.036 nmol/mg/min, CL int of 5.92 ± 0.22, 4.70 ± 0.079, 6.72 ± 0.27 mL/mg/min by RLM, HLM and UGT1A1, respectively. Bilirubin glucuronidation obeyed the Hill equation by RLM and the Michaelis–Menten equation by HLM and UGT1A1 in the range of substrate concentration selected, respectively. In addition, the relative proportions between BDG and BMGs were in connection with enzyme sources (e.g. RLM, HLM and UGT1A1) and bilirubin concentration.
研究领域:
药理学
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生物化学
✓ 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）