JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2017
·
IF 2.603
Tingting Liang,Shun Liu,Fang Wang,Jiamei Gu,Yang Lu,Weike Chen,Cunyu Li,Yunfeng Zheng,Guoping Peng
A specific, sensitive, rapid, precise, and reliable UPLC–MS/MS-based method was designed for the first time for the simultaneous determination of 1-deoxynojirimycin (DNJ) and N-methyl-1-deoxynojirimycin (N-CH 3 -DNJ) in rat plasma. Miglitol was served as the internal standard (IS). An MN-NUCLEODUR HILIC column was assessed to separate the two compounds by isocratic elution using acetonitrile : water with 0.05% formic acid and 6.5 mM ammonium acetate (72:28, v/v) at a flow rate of 0.4 mL/min. A triple quadrupole mass spectrometer was operated in the positive ionization mode using multiple reaction monitoring (MRM), and it was employed to determine transitions of m / z 164.1 → 110.1, 178.1 → 100.1, and 208.1 → 146.1 for DNJ, N-CH 3 -DNJ, and IS, respectively. The method of the two constituents was validated and the results were acceptable. The absolute bioavailability of DNJ and N-CH 3 -DNJ in rats was 50 ± 9% and 62 ± 24%, respectively. The method was then successfully used for the first time to study the pharmacokinetic behavior and absolute bioavailability of DNJ and N-CH 3 -DNJ in rats after intravenous (10 mg/kg) and oral administration (80 mg/kg). The results of this study might provide more information on preclinical pharmacokinetics and a solid basis for assessing the clinical efficacy of DNJ and N-CH 3 -DNJ.
研究领域:
药理学
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分析化学
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药学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Yuzhu Xu,Menghe Huang,Yingting Chen,Lintao Yu,Meiran Wu,Shiyue Kang,Qiuyu Lin,Qiaoxuan Zhang,Liqiao Han,Haibiao Lin,Peifeng Ke,Wenjin Fu,Qizhi Tang,Jun Yan,Xianzhang Huang
Advanced glycation end products (AGEs), derived from the non-enzymatic glycation reaction, are defined as glycotoxins in various diseases including aging, diabetes and kidney injury. Exploring AGEs as potential biomarkers for these diseases holds paramount significance. Nevertheless, the high chemical structural similarity and great heterogeneity among AGEs present a formidable challenge when it comes to the comprehensive, simultaneous, and accurate detection of multiple AGEs in biological samples. In this study, an UPLC/MS/MS method for simultaneous quantification of 20 free AGEs in human serum was firstly established and applied to quantification of clinical samples from individuals with kidney injury. Simple sample preparation method through protein precipitation without derivatization was used. Method performances including imprecision, accuracy, sensitivity, linearity, and carryover were systematically validated. Intra- and inter- imprecision of 20 free AGEs were 1.93–5.94 % and 2.30–8.55 %, respectively. The method accuracy was confirmed with good recoveries ranging from 96.40 % to 103.25 %. The LOD and LOQ were 0.1–3.13 ng/mL and 0.5–6.25 ng/mL, respectively. Additionally, the 20 free AGEs displayed excellent linearity (R 2 >0.9974) across a wide linear range (1.56–400 ng/mL). Finally, through simultaneous quantitation of 20 Free AGEs in 100 participants including kidney injury patient and healthy controls, we identified six free AGEs, including N 6 -carboxyethyl-L-arginine (CEA), N 6 -carboxymethyl-L-lysine (CML), methylglyoxal-derived hydroimidazolones (MG-H), N 6 -formyl-lysine, N 6 -carboxymethyl-L-arginine (CMA), and glyoxal-derived hydroimidazolone (G-H), could well distinguish kidney injury patients and healthy individuals. Among them, the levels of four free AGEs including CML, CEA, MG-H, and G-H strongly correlate with traditionally clinical markers of kidney disease. The high area under the curve (AUC) values (AUC=0.965) in receiver operating characteristic (ROC) curve indicated that these four free AGEs can be served as combined diagnostic biomarkers for the diagnosis of kidney disease.
研究领域:
临床化学
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分析化学
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肾病学
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生物标志物研究
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产品关联
DOI
PubMed
高影响因子
RSC Advances
·
2022
·Vol. 12
·期 15
·9256-9262
·
IF 4.036
Mengmeng Zhao,Xiaoxia Wu,Zengda Yu,Yunkai Sun,Zhao Liu,Jinqiao Yuan,Hu Liu,Yiping Jin
Avanafil is a phosphodiesterase type 5 inhibitor which is used to treat erectile dysfunction in men. The process-related impurities of avanafil were investigated, and four kinds of impurities in several laboratory batches with a content of 0.29–1.63% were detected by the newly developed gradient ultra-high performance liquid chromatography (UPLC). Based on the synthesis route and UPLC-MS research, the impurities are inferred as Imp-A, Imp-B, Imp-C and Imp-D. The structures of the impurities were inferred from LC-MS studies and confirmed by synthesis, followed by spectroscopic characterization such as NMR and mass spectrometry. Especially, the synthesis of Imp-D is firstly reported. The drug-related substances can be separated well by efficient and selective ultra-high performance liquid chromatography on a Waters ACQUITY HSS C18 (50 × 2.1 mm, particle size 1.8 μm) column at 35 °C, with the mobile phase consisting of ammonium formate (20 mM) and acetonitrile, and the detection at 239 nm with a DAD detector. The method was validated in terms of specificity, linearity, precision, accuracy and sensitivity, and satisfactory results were obtained. The results indicated this developed UPLC method for avanafil and the proposed synthesis mechanism can be used for quality control purposes as required by regulatory agencies to ensure the safety and efficacy of the product.
研究领域:
药物化学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
RSC Advances
·
2021
·Vol. 11
·期 37
·23002-23009
·
IF 3.361
Peng Jin,Kai Yang,Ruining Bai,Mei Chen,Shilin Yang,Kebo Fu,Jieli He
Microcystin-LR (MC-LR) generated by cyanobacteria is a kind of potent hepatotoxin, which poses a considerable threat to human health. In the research field of MC-LR removal, the quantitative analysis in a wide concentration range of samples is inevitable. In this paper, we presented the pseudo united use of an Ultra Performance Liquid Chromatography Mass Spectrometry (UPLC-MS) and High Performance Liquid Chromatography system with a Variable Wavelength Ultraviolet Detector (HPLC-VWD) approach to detect MC-LR. The UPLC-MS system was applied to determine MC-LR in trace concentration because of its high sensitivity. However, it is generally believed that the determination of high concentration samples by UPLC-MS will cause problems such as inaccurate quantification and contamination of ion sources. In consequence, the HPLC-VWD was employed to determine the high concentration of MC-LR. The sensitivity, precision and accuracy of the two methods were compared in detail. The linear ranges of UPLC-MS and HPLC-VWD methods were from 0.08 to 10 μg L−1 and 1 to 5000 μg L−1, respectively. The detection and quantification limits of UPLC-MS were 0.03–0.05 μg L−1 and 0.08 μg L−1, and the corresponding two values of HPLC-VWD were 0.6 and 1.0 μg L−1. The recoveries of UPLC-MS and HPLC-VWD were 88.5–106.7% and 98.7–101.6%, with the relative standard deviations of 3.72–5.45% and 0.38–1.69%, respectively. The potential adsorption properties of MC-LR on filter membranes with diverse materials and pore sizes were evaluated and the negative results were obtained. The detection of MC-LR by UPLC-MS was free from matrix effects. The presented UPLC-MS and HPLC-VWD methods were used to analyze the water samples from Erhai Lake, which is located in Dali, Yunnan, China. The results of UPLC-MS analysis indicated that the MC-LR was only identified in water samples of Shuanglang Bay and Xier River, with concentrations of 0.120 and 0.303 μg L−1, whereas MC-LR was not detected by HPLC-VWD.
研究领域:
环境科学
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毒理学
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分析化学
✓ 已验证
DOI
PubMed
高影响因子
ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY
·
2024
·
IF 6.2
Jingyi Tang,Yao Chen,Peng Xue,Yang Chen,Huijun Kong,Cuilan Lin,Xiumin Wang,Shijian Liu
Synthetic steroid hormones are an emerging class of environmental pollutants, but their influence on pubertal timing remains unclear. This case-control study explored the association between synthetic steroid hormone exposure and precocious puberty. Using ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), synthetic steroid hormones were detected in urine samples from 229 Chinese girls, aged 6–9 years. Puberty status was assessed using Tanner staging by professional pediatricians. We conducted the least absolute shrinkage and selection operator (LASSO) regression combined with logistic regression. Besides, we evaluated the joint effects of steroid hormone mixture and identified the main contributor using the Weighted quantile sum (WQS) model and Bayesian kernel machine regression (BKMR) model. The logistic regression model reflected an inverse individual association between precocious puberty and halcinonide [OR (95 %CI): 0.20 (0.07, 0.46)], and budesonide [OR (95 %CI): 0.77 (0.62, 0.95)]. In the joint effects utilizing the WQS model, precocious puberty showed a marginal association with steroid hormone mixture, but was not significant [OR (95 %CI): 0.88 (0.75, 1.04)]. Prednisolone (0.31), fluorometholone acetate (0.24), and dexamethasone acetate (0.12) had the highest weight. Consistently, mixture exposure was not associated with precocious puberty in the BKMR model. In conclusion, precocious puberty was associated with halcinonide and budesonide exposure, but not steroid hormone mixture among girls. It highlighted the management of the residual synthetic steroid hormones in the environment and provided a direction for the prevention of precocious puberty.
研究领域:
内分泌学
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环境健康科学
✓ 已验证
DOI
PubMed
高影响因子
American Journal of Translational Research
·
2024
·Vol. 16
·期 12
·8008
·
IF 1.7
Yalan Zuo,Peidan Yang,Ruixia Yang,Juan Hou,Rui Feng,Ping Liang,Jiang Liu
Objectives: The aim of this study was to establish an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the detection of osimertinib in rat plasma, lung and brain tissues. Methods: Forty-eight rats were randomly divided into an experimental group (receiving osimertinib at doses of 5, 8, and 10 mg/kg) and a control group. After continuous intragastric administration for 15 days, samples of blood, lung, and brain tissue were collected. Chromatographic separation was achieved using a BEH C18 column with gradient elution, employing a mobile phase of water (containing 0.1% (v/v) formic acid) and acetonitrile. The concentration of osimertinib in the samples was determined using an AB SCIEX 5500 triple quadrupole mass spectrometer operated in positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. Results: A UPLC-MS/MS analytical method for determining osimertinib concentrations was successfully established and validated. A linear relationship was observed for osimertinib concentrations in plasma within the range of 1-300 ng/mL, and in lung and brain tissues within the range of 0.5-50 ng/mL. The selectivity, accuracy, precision, matrix effect, extraction recovery, and stability all meet the requirements of methodological validation criteria. Conclusions: A rapid and sensitive UPLC-MS/MS method was developed and validated for quantifying osimertinib concentrations in rat plasma, lung, and brain tissues, providing a valuable tool for pharmacokinetic and tissue distribution studies.
研究领域:
药理学
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分析化学
·
药物代谢动力学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2016
·Vol. 408
·期 10
·2527-2542
·
IF 3.125
Chen Jiahui,Hou Waner,Han Bo,Liu Guanghui,Gong Jin,Li Yemeng,Zhong Danmin,Liao Qiongfeng,Xie Zhiyong
Amino acids, neurotransmitters, purines, and pyrimidines are bioactive molecules that play fundamental roles in maintaining various physiological functions. Their metabolism is closely related to the health, growth, development, reproduction, and homeostasis of organisms. Most recently, comprehensive measurements of these metabolites have shown their potential as innovative approaches in disease surveillance or drug intervention. However, simultaneous measurement of these metabolites presents great difficulties. Here, we report a novel quantitative method that uses hydrophilic interaction ultra-high-performance liquid chromatography–tandem mass spectrometry (HILIC-UPLC–MS/MS), which is highly selective, high throughput, and exhibits better chromatographic behavior than existing methods. The developed method enabled the rapid quantification of 37 metabolites, spanning amino acids, neurotransmitters, purines, and pyrimidines pathways, within 6.5 min. The compounds were separated on an ACQUITY UPLC® BEH Amide column. Serum and brain homogenate were extracted by protein precipitation. The intra- and interday precision of all of the analytes was less than 11.34 %, and the accuracy was between −11.74 and 11.51 % for all quality control (QC) levels. The extraction recoveries of serum ranged from 84.58 % to 116.43 % and those of brain samples from 80.80 % to 119.39 %, while the RSD was 14.61 % or less for all recoveries. This method was used to successfully characterize alterations in the rat brain and, in particular, their dynamics in serum. The following study was performed to simultaneously test global changes of these metabolites in a serotonin antagonist p -chlorophenylalanine (PCPA)-induced anxiety and insomnia rat model to understand the effect and mechanism of PCPA. Taken together, these results show that the method is able to simultaneously monitor a large panel of metabolites and that this protocol may represent a metabolomic method to diagnose toxicological and pathophysiological states.
Overview of experimental workflow
研究领域:
生物化学
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医学
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分析化学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 34
·期 1
·e4703
·
IF 1.748
Shuangshuang Sun,Dongfang Cheng,Shumeng Kong,Xiangping Li,Tongfang Li,Qinglong Yu,Lin Wang
Ibrutinib has an excellent effect in the treatment of mantle cell lymphoma so it has attracted much attention. A novel ibrutinib nanocrystalline was exploited in our study to improve the bioavailability. A fast and reliable UPLC–MS/MS method was established for the accurate quantification of ibrutinib in rat plasma. The chromatographic separation was achieved by an Agilent zorbax SB-C 18 rapid solution HD column (2.1 × 50 mm, 1.8 μm). The mobile phase consisted of deionized water (containing 10 m m ammonium acetate and 0.1% formic acid) and pure acetonitrile. Isocratic elution (water–acetonitrile 10:90, v/v) was adopted and the flow rate was 0.4 mL/min. Column temperature was set to 40°C. Vilazodone was used as the internal standard in this analytical method. Multiple reaction monitoring mode with positive electrospray ionization was selected to detect ibrutinib and vilazodone. Acetonitrile was used to precipitate protein to extract plasma samples. There was no endogenous interference for both ibrutinib and vilazodone and the linear range of this method was 1–2000 ng/mL. The recoveries were 98.4, 97.4 and 102.7% at low, medium and high concentrations. Accordingly, the matrix effect was 96.6, 111.1 and 99.6%. The pharmacokinetic difference between ibrutinib crude and a novel ibrutinib nanocrystalline in rats was investigated by this validated method successfully. The peak concentration and area under the concentration–time curve showed significant differences in gender and the bioavailability was improved after oral administration of ibrutinib nanocrystalline.
研究领域:
药物分析
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药理学
·
生物医学工程
✓ 已验证
DOI
高影响因子
MOLECULES
·
2018
·Vol. 23
·期 2
·459
·
IF 3.098
Ya Song,Xiao-Qun Wei,Mei-Ying Li,Xue-Wu Duan,Yuan-Ming Sun,Rui-Li Yang,Xiang-Dong Su,Ri-Ming Huang,Hong Wang
The aim of this work was to evaluate the main nutrients and their antioxidant properties of a Chinese wild edible fruit,Passiflora foetida,collected from the ecoregion of Hainan province, China. The analytical results revealed thatP. foetidafruits were rich in amino acids (1097 mg/100 g in total), minerals (595.75 mg/100 g in total), and unsaturated fatty acids (74.18 g/100 g in total fat). The lyophilized powder of edible portion contained the higher polyphenols content than the inedible portion powder. The UPLC-Q-TOF-MSEanalysis of the extractable and non-extractable phenolics indicated the presence of 65 compounds including 39 free phenolics, 14 insoluble-glycoside-phenolics, and 22 insoluble-ester-phenolics. In addition, the non-extractable phenolics obtained by alkali hydrolysis showed significant antioxidant activities by/through DPPH and ABTS radical scavenging. These findings ofP. foetidafruits, for the first time, suggest that these polyphenol-rich fruits may have potential nutraceutical efficacies.Keywords:Passiflora foetida;fruit;nutritional composition;antioxidant properties;UPLC-MS;phenolic compound
研究领域:
营养学
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植物化学
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食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2024
·
IF 7.7
Xiao-Jun Li,Shi-Jun Xiao,Yi Heng Xie,Jiang Chen,Hai-Rong Xu,Yuan Yin,Rui Zhang,Tong Yang,Tong-Yu Zhou,Si-Yan Zhang,Pei Hu,Li-Ming Gao,Hui-Ping Peng
An innovative acidic hydrolysate fingerprinting workflow was proposed for the characterization of Lyophyllum Decastes polysaccharide (LDP) by ultra performance liquid chromatography-mass spectrometry (UPLC-MS). The crude polysaccharides were firstly separated and purified by using DE-52 column and the BRT GPC purification system, respectively. The molecular weight and monosaccharide content of homogeneous polysaccharides were ascertained by utilizing HPGPC and ion chromatography separately. Secondly, the linkage of LDP was identified by methylation analysis and 1D/2D NMR spectra. The UPLC-MS/MS was used to scan and identify the acidic hydrolysate products of LDP using the PGC column. The oligosaccharides were collected by chromatography and identified by mass spectrometry. Thirdly, the expression of IL-1β, IL-6, iNOS, TNF-α and IFNAR-I was measured in order to assess the immunological activity of LDP. Besides, the targeted receptors identification of polysaccharides was performed by screening the expression of TLRs family protein. The results showed that oligosaccharide fragments with different molecular weights can be obtained by partial hydrolysis, which further verified that the structures of LDP polysaccharides was a 1–6-linked β-glucan. Moreover, the LDP polysaccharide can up-regulate the content of IL-1β, IL-6, iNOS, TNF-α and IFNAR-I and plays an important immunoregulation role through TLRs family.
研究领域:
生物化学
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免疫学
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产品关联
DOI
PubMed
高影响因子
INDUSTRIAL CROPS AND PRODUCTS
·
2020
·
IF 4.244
Meng Pan,Qicheng Lei,Hong Zhang
Screening of active ingredients in plants is critical for the development of medicinal plants. As a traditional medicinal material, Eucalyptus globulus Labill leaves are regarded as a potential raw material that can be developed as a pesticide because of its original activity. This study proposes a molecular docking assisted UPLC-MS/MS, GC–MS/MS method for the identification and prediction of insecticidal ingredients in the extracts of Eucalyptus globulus leaves. The extracts of Eucalyptus globulus leaves were analyzed by UPLC-MS/MS, GC–MS/MS, 34 aqueous ingredients and 35 volatile ingredients were identified. The identified ingredients were docked with repellent receptor (2KSL). The results showed that protocatechuic acid had strong 2KSL inhibitory activity, which was presumed to be the main reason for the inhibition of 2KSL. Finally, the antifeedant experiment of protocatechuic acid on Henosepilachna vigintioctopunctata (Fabricius) was carried out. The results indicate that the method can effectively screen the active ingredients from the medicinal plants.
研究领域:
植物学
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药理学
·
昆虫学
✓ 已验证
产品关联
DOI
高影响因子
Foods
·
2023
·Vol. 12
·期 15
·2875
·
IF 5.2
Yibo Dong,Xiaolong Yao,Wanping Zhang,Xiaomao Wu
3,4-dichloroaniline (3,4-DCA) and 3,5-dichloroaniline (3,5-DCA) are, respectively, the primary metabolites deriving from the breakdown of phenylurea herbicides and dicarboximide fungicides in both soils and plants, whose residues in vegetable products have a heightened concern considering their higher health risks to humans and greater toxicity than the parent compounds in the environment. In this study, a sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous determination of 3,4-DCA and 3,5-DCA residues in chive products based on the optimization of HPLC-MS/MS chromatographic and mass-spectrometric conditions using the standard substances and the modified QuEChERS preparation technique. The preparation efficiency of 3,4-DCA and 3,5-DCA from chive samples showed that acetonitrile was the best extractant. The combination of the purification agent graphite carbon black + primary secondary amine and the eluting agent acetonitrile + toluene (4:1,v/v) had a satisfactory purification effect. The linear correlation coefficients (R2) were more than 0.996 with the six concentration range of 0.001–1.000 mg/L for 3,4-DCA and 3,5-DCA. The limit of detection and limit of quantitation of this method was 0.6 and 2.0 µg/kg for 3,4-DCA, as well as 1.0 and 3.0 µg/kg for 3,5-DCA, respectively. The matrix effect range of 3,4-DCA and 3,5-DCA in chive tissues was from −9.0% to −2.6% and from −4.4% to 2.3%, respectively. The fortified recovery of 3,4-DCA and 3,5-DCA in chive samples at four spiked levels of 0.001–1.000 mg/kg was 75.3–86.0% and 78.2–98.1%, with the relative standard deviation of 2.1–8.5% and 1.4–11.9%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.6, 2.0, and 1.0, 3.03 for 4-DCA and 3,5-DCA, respectively. This study highlights that the analytical method established here can efficiently and sensitively detect residues of 3,4-DCA and 3,5-DCA residues for monitoring chive products. The method was successfully applied to 60 batches of actual vegetable samples from different regions.Keywords:3,4-dichloroaniline;3,5-dichloroaniline;simultaneous determination;UPLC-MS/MS;chive
研究领域:
分析化学
·
食品安全
·
环境科学
✓ 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）