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.
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FOOD CHEMISTRY
·
2022
·
IF 9.231
Guo-Dong Zhuang,Wen-Ting Gu,Shu-Hong Xu,Dong-Min Cao,Si-Min Deng,Yong-Sheng Chen,Shu-Mei Wang,Dan Tang
A new AAPH-Incubating HPLC-DAD-HR MS/MS method was developed for the rapid and high-throughput screening of antioxidants directly in natural products and applied to Gardenia jasminoides fruit. This method was assumed that the peak areas of compounds with potential antioxidant activity in HPLC chromatograms would be significantly reduced or disappeared after incubating with the AAPH which can release ROO at physiological conditions (37 °C, pH 7.4). Additionally, the activity of antioxidants can be evaluated by comparing the peak reduction rates and the screened components can be further identified by HRMS/MS. Then, 17 potential natural antioxidants from the crude extract of GJF was screened. Among them, three major components including crocin I, crocin II and crocetin showed excellent ROO scavenging activity, which were further validated by the ORAC assay. In conclusion, our study provided a simple and effective strategy to rapidly screen antioxidants in natural products.
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MOLECULES
·
2022
·Vol. 27
·期 21
·7636
·
IF 4.927
Xuyan Fan,Tao Tang,Song Du,Ningning Sang,Hao Huang,Chenghui Zhang,Xueping Zhao
A rapid, efficient, simple, and high-throughput method for the simultaneous determination of 108 pesticide residues in three traditional Chinese medicines (TCMs) was established, comprising an improved QuEChERS method in combination with HPLC-MS/MS based on mixed samples. A quantity of 10 mL of acetonitrile was used as extraction solvent, and 10 mg of amino-modified multi-walled carbon nanotubes (MWCNTs-NH2) and 150 mg of anhydrous magnesium sulfate (MgSO4) were selected as sorbents for dispersive solid phase extraction. The performance of the method was verified according to the analytical quality control standards of SANTE/11813/2017 guidelines. With good linearity (R2> 0.9984) in the range of 2–200 μg/L for all pesticides in the selected matrices, and good accuracy, precision, and high sensitivity, the recoveries were in the range of 70–120% for more than 95% of the pesticides, with a relative standard deviation (RSD) of less than 16.82% for all. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.01–3.87 μg/kg and 0.07–12.90 μg/kg, respectively, forFritillaria thunbergiiMiq (F. thunbergii),Chrysanthemum MorifoliumRamat (C. morifolium), andDendrobium officinaleKimura et Migo (D. officinale). The method was successfully applied to 60 batches of actual samples from different regions.Keywords:pesticide residue;QuEChERS;MWCNTs-NH2;traditional Chinese medicines
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ANALYTICAL LETTERS
·
2022
·
IF 2.267
Ru Li,Xuan Zou,Pan Luan,Xiaokun Liu,Ning Wang,Qian Wang,Huashi Guan,Zhe Xu
Thrombosis is the main cause of many cardiovascular diseases. The conventional pharmaceuticals used for preventing thrombosis can induce significant adverse side effects, especially bleeding risk. Hence, the development of more effective and safe antithrombotic agents is strongly demanded to improve clinical treatment. In order to rapidly screen and identify novel antithrombotic substances from natural marine products, a multi-target screening strategy is reported to quantify the antithrombotic activity with high-performance liquid chromatography – mass spectrometry (HPLC-MS). Five key thrombosis-related targets, including thrombin, coagulation factors Xa, XIa and XIIa and platelet phosphodiesterase 3, were selected to establish the multi-target antithrombotic activity screening assay. The Michaelis-Menten constants (Km) were 8.16 µM, 58.85 µM, 120.03 µM, 35.24 µM and 79.67 µM, respectively. Five known inhibitors, namely argatroban, rivaroxaban, benzamidine, 3-carboxamide-coumarinand, and milrinone, were used for validation. The reproducibility of the screening strategy was verified by calculating the overall average Z′ value, which was 0.88. Subsequently, this method was assessed by screening a small marine library of 78 compounds. Five coumarin compounds were selected, and their antithrombotic activities were further validated in standard assessments of enzyme inhibition and on the coagulometer. According to the validation, the multi-target assay based on dried blood spots and HPLC-MS was suitable for screening antithrombotic substances with considerable reliability.
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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.
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MOLECULES
·
2022
·Vol. 27
·期 7
·2088
·
IF 4.927
Xue-Li Liu,Yong-Hui Wang,Shu-Yue Ren,Shuang Li,Yu Wang,Dian-Peng Han,Kang Qin,Yuan Peng,Tie Han,Zhi-Xian Gao,Jian-Zhong Cui,Huan-Ying Zhou
The efficient capture of multi-pollutant residues in food is vital for food safety monitoring. In this study, in-situ-fabricated magnetic MIL-53(Al) metal organic frameworks (MOFs), with good magnetic responsiveness, were synthesized and applied for the magnetic solid-phase extraction (MSPE) of chloramphenicol, bisphenol A, estradiol, and diethylstilbestrol. Terephthalic acid (H2BDC) organic ligands were pre-coupled on the surface of amino-Fe3O4composites (H2BDC@Fe3O4). Fe3O4@MIL-53(Al) MOF was fabricated by in-situ hydrothermal polymerization of H2BDC, Al (NO3)3, and H2BDC@Fe3O4. This approach highly increased the stability of the material. The magnetic Fe3O4@MIL-53(Al) MOF-based MSPE was combined with high-performance liquid chromatography-photo diode array detection, to establish a novel sensitive method for analyzing multi-pollutant residues in milk. This method showed good linear correlations, in the range of 0.05–5.00 μg/mL, with good reproducibility. The limit of detection was 0.004–0.108 μg/mL. The presented method was verified using a milk sample, spiked with four pollutants, which enabled high-throughput detection and the accuracies of 88.17–107.58% confirmed its applicability, in real sample analysis.Keywords:magnetic metal organic framework (MMOFs);magnetic solid-phase extraction (MSPE);multi-pollutants;high-performance liquid chromatography (HPLC)
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Journal of Food Measurement and Characterization
·
2021
·Vol. 15
·期 5
·3873-3883
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IF 2.431
Qian Zheng-ming,Huang Qi,Feng Xiao-long,Li De-qiang
Given the safety of synthetic antioxidants, people are increasingly inclined to develop and use natural antioxidants. However, rapid screening and identification of active ingredients from the complex systems of natural products is one of the major challenges for the modernization of traditional Chinese medicine. In this study, online extraction-high performance liquid chromatography-diode array detection-quadrupole time-of-flight mass spectrometry coupled with ABTS antioxidant assay (OLE-HPLC-DAD-QTOF-MS/MS-ABTS), in which sample preparation, separation, detection and antioxidant assay were integrated in a single step, was used to rapidly identify antioxidant components from the different parts of Citrus reticulata , including its peels, leaves, vascular bundies and seeds. After method validation (system adaptability, extraction yield and repeatability), the four samples of different botanical parts were analyzed. As a result, among 49 found chromatographic peaks, 33 peaks displayed varying degrees of antioxidant activity and 39 peaks were tentatively or unambiguously identified based on their retention time, UV spectrum and mass spectrometry information and the comparison with reference substance and data in literature, including 10 phenolic acids, 9 polymethoxy flavonoids, 7 flavonoid- O -glycosides and 13 other ingredients. It is concluded that the established method is simple, fast, and reliable, which not only saves the materials and solvents as well as time, but also reduces the risk of degradation of chemical components during the extraction process, suitable for rapid screening and identification of antioxidant components of complex mixture.
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Dose-Response
·
2020
·
IF 2.438
Zhang Qian,Chen Yiyang,Ma Lixia,Jiang Yue,Chen Jun,Dong Jie,Ma Yifan,Zhang Jingjing,Yan Guojun
Objective:To establish a HPLC fingerprints evaluation method for Angelica Sinensis Radix (ASR) based on traditional decoction process of Ancient Classical Prescriptions of Traditional Chinese Medicine (ACPTCM).Methods:The fingerprints of 10 batches of ASR were further evaluated by chemometrics methods. The similarity analyzed with “Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine 2004A,” and hierarchical clustering analysis (HCA) and principal component analysis (PCA) were performed by SPSS (version 22.0, SPSS Inc., Chicago, IL, USA).Results:There were 12 common peaks, and the similarity degrees of 10 batches of samples were more than 0.923 and showed that all the samples from different origins were of good consistency. The samples were divided into 4 clusters by HCA. The results of PCA showed that the 3 factors were chosen, the quality of samples could be evaluated basically. The comprehensive score results show that the ASR with Lot.Nos.DG-18007, DG-18008 in Weiyuan County, Gansu and DG-18009 produced in Minle County, Gansu Province rank among the top 3 in all samples.Conclusions:These results demonstrated that the combination of HPLC chromatographic fingerprint and chemometrics offers an efficient and reliable approach for quality evaluation of ASR from different sources as Ancient Classical Prescriptions ingredients.
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PHARMACEUTICAL BIOLOGY
·
2021
·
IF 3.503
Cai-Yun Zhang,Ya-Ting Lu,Yin-Feng Tan,Qi-Bing Liu,Lin Dong,Ning Ma,Wei-Ying Lu,Zhi-Heng Su,Xiao-Po Zhang
Context Tadehaginoside, an active ingredient isolated from Tadehagi triquetrum (Linn.) Ohashi (Leguminosae), exhibited various biological activities. However, the pharmacokinetics and tissue distribution which affect tadehaginoside’s therapeutic actions and application remain elusive.Objective To clarify the metabolism of tadehaginoside in vivo.Materials and methods The pharmacokinetics and tissue distribution of tadehaginoside and its metabolite p-hydroxycinnamic acid (HYD) were investigated using LC-MS/MS. Pharmacokinetic parameters were determined in 10 Sprague-Dawley rats divided into two groups, the intravenous group (5 mg/kg) and the oral group (25 mg/kg). For the tissue-distribution study, 20 rats were intravenously given tadehaginoside (5 mg/kg) before the experiment (n = 4). Biological samples were collected before drug administration (control group) and after drug administration.Results The linearity, accuracy, precision, stability, recovery and matrix effect of the method were well-validated and the results satisfied the requirements of biological sample measurement. Treatment with tadehaginoside via intragastric and intravenous administration, the calculated Cmax in rats was 6.01 ± 2.14 ng/mL and 109.77 ± 4.29 ng/mL, and Tmax was 0.025 ± 0.08 h and 0.08 h, respectively. The results indicated that the quick absorption of tadehaginoside was observed following intravenous administration, and tadehaginoside in plasma of rats with intragastric administration showed relatively low concentration may be due to the formation of its metabolite. Tissue-distribution study indicated that kidney and spleen were the major distribution organs for tadehaginoside in rats and there was no long-term accumulation in most tissues.Discussion and conclusion These results could provide clues for exploring the bioactivity of tadehaginoside based on its pharmacokinetic characteristics.
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Analytical Methods
·
2020
·Vol. 13
·期 5
·636-641
·
IF 2.596
Beiqi Wu,Zhengyan Guo,Xiuting Li,Xin Huang,Chao Teng,Zhenjia Chen,Xu Jing,Wenting Zhao
This work presents a novel and green analytical procedure involving a deep eutectic solvent-based dispersive liquid–liquid microextraction with solidification of floating organic droplets (DES-DLLME-SFOD) followed by HPLC to measure three pyrethroids (bifenthrin, β-cypermethrin, and deltamethrin) in cereal samples. Firstly, a low-density hydrophobic DES was synthesized from thymol and octanoic acid in the molar ratio of 1/4 and this was applied as a green extraction solvent in the DLLME procedure to avoid the use of a toxic extractant. After centrifugation and placing it on an ice bath, it is transformed into a solid phase on the top of the sample solution to reduce the loss of extractant, conducive to convenient collection thereafter. This procedure required the optimal conditions (including the type, proportion, and amount of DES as the extractant, the volume of the dispersant acetonitrile, the amount of salt, and the pH value) to be evaluated. Under optimized variates, the proposed method provided good linearity with a correlation coefficient greater than 0.997 and limits of quantification within the range of 6.6–8.9 μg kg−1. The recoveries of pyrethroids in corn, wheat, barley, and oats were 75.6–87.2%, and the relative standard deviation was less than 3.6%. The method, therefore, offers a green, efficient, and convenient approach for the determination of pesticides in cereals.
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JOURNAL OF INTERNATIONAL MEDICAL RESEARCH
·
2020
·
IF 1.287
Yulong Gu,Xianglan Piao,Dan Zhu
ObjectiveThis study aimed to develop and validate a high-performance liquid chromatography–tandem mass spectrometry method to simultaneously determine three bioactive components of the Huangqi Chifeng decoction (HQCF) in rat plasma.MethodsTaxol was used as an internal standard in the developed method. Chromatographic separation was performed on a C18 column using a gradient elution with 0.1% formic acid in acetonitrile (v/v) and 0.1% formic acid in water (v/v) as the mobile phases at a flow rate of 0.4 mL·minute−1. All compounds were monitored via selected reaction monitoring with an electrospray ionization source.ResultsThe lower limits of quantification of paeoniflorin, calycosin, and prim-O-glucosylcimifugin were 15.0, 0.75, and 0.75 ng·mL−1, respectively. The calibration curves indicated optimal linearity (r > 0.99) across the concentration ranges. The specificity, precision, accuracy, recovery, matrix effect, and stability of the method were validated. This method was successfully applied in a pharmacokinetics study of the three compounds in rat plasma.ConclusionThe pharmacokinetics results provide insights into the mechanisms of HQCF in vivo and its future clinical application.
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JOURNAL OF SEPARATION SCIENCE
·
2020
·Vol. 43
·期 14
·2827-2833
·
IF 2.878
Zichun Liu,Wei Zhou,Chenlu Wang,Wei Hu,Zilin Chen
Cotton fiber is a biodegradable material that possesses properties such as high specific area, adjustable shape, and hygroscopicity. In this work, organic polymer was directly in situ grown on the surface of cotton thread and packed into a poly(ether ether ketone) tube for online in-tube solid-phase microextraction. The novel strategy solves the problems like high backpressure and tedious optimization process of normal monolithic polymer-based in-tube solid-phase microextraction capillary. The quaternary ammonium typed ionic liquid of 1-allyl-methylimidazolium chloride, 4-vinylbiphenyl, and ethylene dimethacrylate were co-polymerized and in situ grown on the surface of cotton thread as extraction phase. The solid-phase microextraction tube showed excellent performance for the extraction of three nonsteroidal anti-inflammatory drugs including ketoprofen, naproxen, and flurbiprofen due to the strong ion exchange and hydrophobic interactions. After online coupling with a high-performance liquid chromatography system by six-port valve, the method was applied for the quantitative analysis of nonsteroidal anti-inflammatory drugs in human plasma samples showing good enrichment performance (enrichment factor between 263 and 279), high sensitivity, good linearity, and good reproducibility.
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