JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2015
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IF 2.979
Lu Zhang,Jun-qing Yang,Ying Luo,Jing-chuan Shang,Xin-hui Jiang
A simple and rapid high-performance liquid chromatography method with electrochemical detection employing boron-doped diamond electrode (BDD) was established for simultaneous determination of eleven bioamines with their precursor amino acids and metabolites, including two precursors (tyrosine and tryptophan), three catecholamines (dopamine, norepinephrine and epinephrine) and their four metabolites (3,4-dihydroxyphenylacetic acid, 3-methoxytyramine, homovanillic acid, and 3-methoxy-4-hydroxyphenylglycol), as well as serotonin and its metabolite (5-hydroxyindoleacetic acid), in a single run of 20 min using vanillic acid as internal standard. The separation was performed on an ODS2 column (250 mm × 4.6 mm, 5.0 μm) with column oven temperature of 30 °C. Quantification was accomplished at an oxidation potential of 700 mV vs Ag/AgCl reference electrode after a range of applied voltages were tested. Several parameters of this new chromatographic method were validated after optimizaton of the analytical conditions. The new method was successfully applied to test cortex and hippocampus samples from Sprague-Dawley rats with good separation. These eleven compounds in cortices and hippocampi were compared, which was used for monitoring their variations in neuroscience research.
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JOURNAL OF PHARMACOLOGICAL SCIENCES
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2015
·
IF 2.36
Fang Li,Yi-Sha Tan,Hong-Lin Chen,Yan Yan,Ke-Feng Zhai,Da-Peng Li,Jun-Ping Kou,Bo-Yang Yu
YiQiFuMai Powder Injection (YQFM) is a re-developed preparation based on the well-known traditional Chinese medicine formula Sheng-mai-san. It has been widely used for the treatment of cardiovascular disease with definite clinical efficacy in China, but its bioactive molecules remain obscure. In this study, an effective method has been employed as a tool for screening active components in YQFM, using human umbilical vein endothelial cells (HUVECs) extraction and liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (Q-TOF MS/MS). Nine compounds, which could interact with HUVECs, were identified as ginsenosides Rb1, Rc, Rb2, Rd, 20(S)-Rg3, 20(R)-Rg3, Rk1/Rg5 and schisandrin by comparing with reference substances or literature. In vitro assays showed that schisandrin at concentrations of 10–100 μM protected HUVECs from hypoxia/reoxygenation (H/R) injury, increased cell viability, nitric oxide (NO) content and decreased lactate dehydrogenase (LDH) leakage, malonaldehyde (MDA) content and ROS generation. Moreover, schisandrin pretreatment inhibited cell apoptosis, as evidenced by inhibiting activation of caspase-3 and increasing the Bcl-2/Bax ratio. These data indicate that HUVECs biospecific extraction coupled with HPLC-ESI-Q-TOF-MS/MS analysis is a reliable method for screening potential bioactive components from traditional Chinese medicines. Meanwhile, the vascular endothelium protective property of schisandrin might be beneficial for the treatment of cardiovascular disease.
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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2013
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IF 2.906
Zhixiong Hu,Peng Cheng,Mingli Guo,Weinong Zhang,Yutang Qi
A novel approach of periodate oxidation coupled with high-performance liquid chromatography (HPLC)–fluorescence detection (FLD) for the quantitative determination of 3-chloro-1,2-propanediol (3-MCPD) has been established. The essence of this approach lies in the production of chloroacetaldehyde by the oxidization cleavage of 3-MCPD with sodium periodate and the HPLC analysis of chloroacetaldehyde monitored by an FLD detector after fluorescence derivatization with adenine. The experimental parameters relating to the efficiency of the derivative reaction such as concentration of adenine, chloroacetaldehyde reaction temperature, and time were studied. Under the optimized conditions, the proposed method can provide high sensitivity, good linearity (r2 = 0.999), and repeatability (percent relative standard deviations between 2.57% and 3.44%), the limits of detection and quantification were 0.36 and 1.20 ng/mL, respectively, and the recoveries obtained for water samples were in the range 93.39–97.39%. This method has been successfully applied to the analysis of real water samples. Also this method has been successfully used for the analysis of vegetable oil samples after pretreatment with liquid–liquid extraction; the recoveries obtained by a spiking experiment with soybean oil ranged from 96.27% to 102.42%. In comparison with gas chromatography or gas chromatography–mass spectrometry, the proposed method can provide the advantages of simple instrumental requirement, easy operation, low cost, and high efficiency, thus making this approach another good choice for the sensitive determination of 3-MCPD.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2016
·
IF 3.169
Yidi Yang,Xi Zhu,Fei Zhang,Wei Li,Ying Wu,Li Ding
Stress testing was carried out under acidic, alkaline, oxidative, thermal and photolytic conditions to evaluate the intrinsic stability of posaconazole injection. A total of four degradation products were detected and the drug was found to be susceptible to oxidative and thermal degradations. Three unknown degradants formed under oxidative stress condition were isolated by preparative HPLC and unambiguously elucidated by LC–TOF/MS, LC–MS/MS, 1 H NMR, 13 C NMR and 2D NMR techniques. Based on the spectrometric and spectroscopic information, these novel degradation products were unequivocally assigned as the N-oxides of posaconazole. Probable mechanisms for the formation of the degradants were proposed. A new and selective HPLC method was developed and validated to separate, detect and quantify all the degradants in posaconazole injection.
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JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Xue Li,Meng-Yao Wang,Yu Wang,Wen-Zhi Yang,Cheng-Xiong Yang
Efficient enrichment of trace zearalenone (ZEN) from the complex traditional Chinese medicine (TCM) samples is quite difficult, but of great significance for TCM quality control. Herein, we reported a novel magnetic solid phase extraction (MSPE) strategy for ZEN enrichment using the amino- and hydroxyl dual-functionalized magnetic microporous organic network (Fe 3 O 4 @MON-NH 2 -OH) as an advanced adsorbent combined with the high-performance liquid chromatography (HPLC) determination. Efficient extraction of ZEN was achieved via the possible hydrogen bonding, hydrophobic, and π-π interactions between Fe 3 O 4 @MON-NH 2 -OH and ZEN. The adsorption capacity of Fe 3 O 4 @MON-NH 2 -OH for ZEN was 215.0 mg g −1 at the room temperature, which was much higher than most of the reported adsorbents. Under the optimal condition, the developed Fe 3 O 4 @MON-NH 2 -OH-MSPE-HPLC method exhibited wide linear range (5–2500 μg L −1 ), low limits of detection (1.4–35 μg L −1 ), less adsorbent consumption (5 mg), and large enhancement factor (95) for ZEN. The proposed method was successfully applied to detect trace ZEN from 10 kinds of real TCM samples. Conclusively, this work demonstrates the Fe 3 O 4 @MON-NH 2 -OH can effectively extract trace ZEN from the complex TCM matrices, which may open up a new way for the application of MONs in the enrichment and extraction of trace contaminants or active constituents from the complex TCM samples.
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Science China-Chemistry
·
2018
·Vol. 61
·期 6
·739-749
·
IF 4.448
Wang Tong,Wu Hai-Long,Xie Li-Xia,Liu Zhi,Long Wan-Jun,Cheng Li,Ding Yu-Jie,Yu Ru-Qin
In this work, a smart strategy that combines three-way high performance liquid chromatography-diode array detection (HPLCDAD) data with second-order calibration method based on alternating trilinear decomposition (ATLD) algorithm was proposed for simultaneous determination of eleven non-steroidal anti-inflammatory drugs (NSAIDs) illegally added into Chinese patent drugs and health products. All target analytes were rapidly eluted out within 14.5 min under a simple gradient elution. With the aid of the prominent “second-order advantage” of the ATLD algorithm, three HPLC problems, i.e. peak overlaps, unknown interferences and baseline drift, could be mathematically calibrated, and pure signals of target analytes could be extracted out from heavy-interference but information-rich HPLC-DAD data. The average spiked recoveries for all target analytes were in the range of 95.9%–106.4% with standard deviations lower than 7.5%. Validation parameters including sensitivity (SEN), selectivity (SEL), limit of detection (LOD), limit of quantitation (LOQ) and precisions of intra-day and inter-day were calculated to validate the accuracy of the proposed method, quantitative results were further confirmed by the classic HPLC method, which proved that chemometrics-assisted HPLC-DAD analytical strategy was highly efficient, accurate and green for drug-abuse monitoring of NSAIDs in Chinese patent drugs and health products.
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MICROCHEMICAL JOURNAL
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2024
·
IF 4.9
Guanghou Wang,Xueqian Tang,Feixu Qin,Hongjin Wang,Hao Zhang,Hanyue Li,Lan Wei,Lixin Sun
Nauclea officinalis ( N. officinalis ), a medicinal plant of the genus Nauclea in the Rubiaceae family, is used to treat bronchitis, pneumonia and acute tonsillitis and enteritis in China. Extracts of N. officinalis include more than 60 alkaloids, which exert all kinds of pharmacological effects, such as antiproliferative, antiparasitic, antimicrobial, anticancer, and anti-inflammatory activities. In this study, an affinity ultrafiltration and high-performance liquid chromatography- tandem mass spectrometry (AUF-LC-MS/MS) approach was constructed and validated, and was applied to rapidly screen COX-2/5-LOX inhibitors in N. officinalis extracts (NOE). To gain a more comprehensive and profound understanding of the anti-inflammatory mechanism of N. officinalis . Central Composite Design (CCD) of Response Surface Method (RSM) was used to optimize extraction conditions for potential COX-2/5-LOX inhibitors from NOE. Next, COX-2/5-LOX dual targeted inhibitors were screened from NOE using AUF-LC-MS/MS, and the biological activity of the screened ligands was demonstrated by enzyme inhibition assay. Finally, the preferred binding modes for these COX-2/5-LOX inhibitors were then determined by molecular docking, and compared with active drugs celecoxib and zileuton, respectively, to further explore ligand active binding sites and intersections between ligands and target proteins. The optimum extraction conditions were follows: ethanol concentration of 79 %, liquid − solid ratio of 11.8 v / w and extraction time of 1.8 h. The results of COX-2 inhibition assay showed that angustine (AU) had the more stronger inhibition activity with an IC 50 of 20.49 μM, followed with IC 50 of angustidine (AD) and nauclefine (NF) were 35.89 and 60.45 μM, respectively. Among the three components, AU also exhibited the highest inhibition of 5-LOX with an IC 50 of 1.18 μM, followed by NF and AD at 2.75 and 4.35 μM, respectively. Owing to the synergistic effect of multiple components make NOE exhibit strong inhibitory activity, it is shown potent inhibitory activities with an IC 50 at 9.47 and 6.16 μg/mL for COX-2 and 5-LOX, respectively. This work has demonstrated that NF, AD, and AU are potential COX-2/5-LOX dual-target inhibitors, indicating that N. officinalis anti-inflammatory activities were partially based on these COX-2/5-LOX inhibitors. These research results can also be further used for developed or improved anti-inflammatory agents with more beneficial effects.
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FOOD CHEMISTRY
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2024
·
IF 8.5
Hua Wang,Lin Hao,Yaxing Guo,Chun Wang,Qiuhua Wu,Zhi Wang
Porous electron-rich organic frameworks have attracted an increased attention in the adsorption and removal of pollutants due to their abundant electron-rich nitrogen atoms, which can effectively interact with positively charged substance. In this study, a porous electron-rich organic framework (Car-POF) and positively charged amino-functionalized magnetic nanoparticles (Fe 3 O 4 -NH 2 ) were used to construct a magnetic electron-rich Fe 3 O 4 -NH 2 @Car-POF for the enrichment of some phenylurea herbicides from water and milk samples prior to high performance liquid chromatographic detection. The adsorption capacity of Fe 3 O 4 -NH 2 @Car-POF for the phenylureas ranged from 14.93 to 28.83 mg g −1 . The LODs were observed in the range of 0.05–0.20 ng mL −1 and 0.5–1.5 ng mL −1 , and LOQs in the range of 0.17–0.66 ng mL −1 and 1.7–5.0 ng mL −1 for water and milk samples with RSD less than 9.0. The adsorption studies with cationic and anionic dyes revealed that Fe 3 O 4 -NH 2 @Car-POF is favorable for the adsorption of positively charged compounds.
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BIOMEDICAL CHROMATOGRAPHY
·
2024
·
IF 1.8
Yonglin Ma,Yue Zhang,Yu Zhao,Jiwen Wang,Qianqian Hu,Lianlin Yang,Shuzhen Chen,Yong Diao,Hongliang Ma
In this study, an online antioxidant assay based on HPLC-ABTS was mainly developed for screening the antioxidants of flavonoids from Astragali Radix (AR), and comparing the antioxidant capacity between traditional decoction pieces (TDP) of AR and cell wall-broken decoction pieces (CDP) of AR. The experimental results showed that the overall antioxidant capacity of CDP of AR was about twice as much as that of TDP of AR, which was specifically expressed as the antioxidant capacity of the screened antioxidants extracted from CDP was equivalent to 1.9–5.1 times that of those extracted from TDP, and three antioxidants were successfully screened, which were calycosin-7-O-β-D-glucoside, calycosin, and formononetin. The method established in this study is characterized by high efficiency and accuracy, which can simultaneously accomplish the screening of antioxidant components and the comparison of antioxidant capacity between samples, and provides a new method for the quality evaluation of AR from the perspective of antioxidant activity.
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MICROCHEMICAL JOURNAL
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2024
·
IF 4.9
Linzhou Chen,Jiedan Zhou,Yuesen shi,Fei Xu,Xin Liu,Qingda Huang,Jinjian Zhong,Ke Wu,Dafeng Yang,Huajun Fan,Xiangliang Yang
Collecting exhaled breath aerosols (EBA) as a sample has a great potential to monitoring illicit drug abuse due to advantages of simple, non-invasiveness and unrestricted sampling. However, scarcity of positive samples has cramped development of more efficient techniques for monitoring illicit drug abuse in EBA. In this work, a simulated human exhaled breath aerosol (SHEBA) generating device based on Venturi jet principle was constructed by integrating nebulizing unit and collection unit to prepare positive EBAs. By means of ultra high-performance hyphenated with triple quadrupole tandem mass spectrometry (HPLC-TQ-MS/MS), using caffeine as a target drug, the device parameters were investigated by studying the effects of flow rates of nebulizing and auxiliary gases, drug concentration and etc., the performance was further validated by commonly abused drugs such as amphetamines (AMP, MAMP, MDA and MDMA). Electret material as adsorbent was used to collect SHEBAs generated by the device, achieving HPLC-TQ-MS/MS detection of the captured drugs at 40.0–2000.0 pg/filter. By this way, caffeine content in EBAs from six volunteers was successfully detected in the range of 51.6 ± 6.8–708 ± 51 pg/filter after drinking the caffeinated beverage. These validation experiments proved that SHEBA generating device could not only meet to the requirement of EBA analysis for illicit drug abuse at trace levels, but also provide the correction factors to calibrate the lower detection value caused by incomplete material adsorption.
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Food Chemistry-X
·
2025
·
IF 8.2
Binbin Li,Qian Mu,Huijing Guo,Wenting Jia,Mengzhen Zhang,Ya Liu,Xinwen Jin
The effects of jujube pretreatment at different roasting temperatures (80–160 °C) on the dynamic changes in free amino acids and volatile organic compounds in jujube wine were evaluated using HPLC, HS-GC-IMS, HS-SPME-GC–MS, and sensory analysis. The results revealed that roasting at 80–100 °C enhanced the accumulation of sweet amino acids in jujube wine, whereas roasting at 140–160 °C increased the bitter amino acid content. As the roasting temperature increased, the contents of esters, alcohols, acids, aldehydes, and ketones in jujube wine rose initially before declining thereafter. Meanwhile, the furan compound content exhibited a continuous increase. Through multivariate statistical analyses, including orthogonal partial least squares-discriminant analysis (OPLS-DA), relative odor activity value (ROAV) calculations, and variable importance in projection (VIP), six key characteristic flavor compounds were identified. These included isoamyl acetate, ethyl hexanoate, and ethyl octanoate. The novel insights derived from this study could guide the improvement of jujube wine flavor.
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JOURNAL OF SEPARATION SCIENCE
·
2025
·Vol. 48
·期 2
·e70090
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IF 2.8
Han Li,Xiaoming Wu,Yan Miao,Fengyu Dong,Xinjing Gui,Panpan Wang,Xuelin Li,Ruixin Liu
This study investigates the consistency of quality between the traditional decoction (TD) of Pheretima aspergillum and its dispensing granule decoction (DGD) by examining their chemical composition and antithrombotic efficacy. We first determined the nucleoside components, protein content, and volatile compounds in 10 batches of TD and 9 batches of DGD sourced from three manufacturers using high-performance liquid chromatography (HPLC), UV–vis spectrophotometry, and gas chromatography ion mobility spectrometry (GC-IMS). Next, we assessed antithrombotic efficacy by measuring the relative length of tail thrombosis and calculating the thrombus inhibition rates at 24 and 48 h. Our comprehensive analysis revealed that the concentrations of hypoxanthine, uridine, inosine, adenosine, and proteins in TD were significantly higher than those in DGD. Moreover, the types and concentrations of volatile compounds in TD and DGD exhibited substantial differences, with 19 volatile compounds identified as differentially present between the two decoctions. Despite these compositional differences, both decoction types demonstrated equivalent antithrombotic efficacy. Overall, the quality of DGD from manufacturers A and B aligned closely with that of TD. However, TD exhibited a higher overall quality compared to DGD, while both decoctions maintained consistent antithrombotic efficacy.
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