INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
·
2022
·Vol. 23
·期 15
·8810
·
IF 6.208
Ting Xue,Wenqing Wang,Zhiyuan Yang,Fanjun Wang,Lei Yang,Jian Li,Hui Gan,Ruolan Gu,Zhuona Wu,Guifang Dou,Zhiyun Meng
The mole fraction of deacetylated monomeric units in chitosan (CS) molecules is referred to as CS’s degree of deacetylation (DD). In this study, 35 characteristic ions of CS were detected using liquid chromatography–electrospray ionization–mass spectrometry (LC–ESI–MS/MS). The relative response intensity of 35 characteristic ion pairs using a single charge in nine CS samples with varying DDs was analyzed using 30 analytical methods. There was a good linear relationship between the relative response intensity of the characteristic ion pairs determined using ultrahigh performance (UP) LC–MS/MS and the DD of CS. The UPLC–MS/MS method for determining the DD of CS was unaffected by the sample concentration. The detection instrument has a wide range of application parameters with different voltages, high temperatures, and gas flow conditions. This study established a detection method for the DD of CS with high sensitivity, fast analysis, accuracy, stability, and durability.Keywords:chitosan;degree of deacetylation determination;UPLC–MS/MS;relative response intensity of the characteristic peak
研究领域:
生物化学
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分析化学
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DOI
PubMed
高影响因子
Journal of Materials Chemistry B
·
2021
·Vol. 9
·期 14
·3192-3199
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IF 6.331
Yuanchen Liu,Yujian Liu,Zhiming Liu,Jonathan P. Hill,Azhar Alowasheeir,Zhigang Xu,Xingtao Xu,Yusuke Yamauchi
Traditional analysis methods are susceptible to interference caused by the complexity of sample matrices, and detector surface fouling arising from nonspecific adsorption of microorganisms (in biological samples) which leads in particular to a gradual loss of sensitivity. Imprinted materials can be used to effectively reduce interference originating in the matrices. However, the poor reproducibility and multicomponent quantification of trace antibiotics represent significant challenges to the detection process. Meanwhile, the high biological risk presented by bacterial antibiotic immunity and the persistence of antibiotics in foodstuffs, especially meat, both caused by the overuse of sulfonamide antibiotics, remain urgent issues. Here, we present the first example of a method for the accurate quantification of trace sulfa antibiotics (SAs) based on multi-template imprinted polymers (MMIPs). Levels of multiple SAs have been simultaneously successfully quantified by applying MMIP extraction coupled with UPLC-MS/MS analysis. This method shows excellent linearity of detection in the range of 0.1–500 μg L−1, and ultrasensitivity with low limits of detection of 0.03 μg L−1. The maximum SA residue recovered from sample tissues by using MMIPs was 5.48 μg g−1. MMIP-coupled UPLC-MS/MS quantification of SAs is an accurate and repeatable method for the monitoring of SA accumulation in mouse tissue samples. It also provides an effective strategy for the tracking and quantification of drugs in other biological samples.
研究领域:
分析化学
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环境科学
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食品安全
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DOI
PubMed
高影响因子
TALANTA
·
2024
·
IF 5.6
Yifan Liu,Zihui Jin,Di Sun,Jiexin Zheng,Bo Xu,Tianyu Lan,Qiyang Zhao,Yue He,Jing Li,Yaohai Zhang,Yongliang Cui
Both rhoifolin and diosmin belong to flavonoids, which are widely present in citrus. Diosmin is not only used in the medical field in the world, but also used as a dietary supplement in the United States. Rhoifolin has a similar structure to diosmin and also exhibits antioxidant and anti-inflammatory properties. In this study, an anti-rhoifolin monoclonal antibody was prepared and an indirect competitive enzyme-linked immunosorbent assay (icELISA) method was established. The half-maximal inhibitory concentration (IC 50 ) of icELISA was determined to be 4.83 ng/mL, and the detection range was 0.97–33.87 ng/mL. The results of UPLC-MS/MS and icELISA generally demonstrate consistency. Moreover, by exploiting the cross-reactivity of the antibody, diosmin in tablets can be detected by icELISA. The results demonstrate that the developed method has good accuracy, reproducibility, and broad application prospects.
研究领域:
药理学
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分析化学
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免疫学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 6
·e4193
·
IF 1.688
Ping Guo,Jingjing Zhang,Xiaohui Chen,Longshan Zhao
A molecularly imprinted polymer was synthesized and applied as a sorbent in the solid-phase extraction device. The imprinted polymer was characterized by fourier-transform infrared spectroscopy and scanning electron microscope. The results revealed that imprinted polymer possess sensitive selectivity and reliable adsorption properties for five NSAIDs. The imprinted polymer was successfully applied to the pre-concentration for five NSAIDs in different water samples prior to UPLC-MS/MS. In the early studies, several factors were investigated, including pH adjustment, the kind of elution solvent and the volume of elution solvent. Finally, we found that the pH 5 and an aliquot of 2 mL methanol were suitable for the water samples. The limits of detection and limits of quantitation of five nonsteroidal anti-inflammatory drugs varied from 0.007 to 0.480 μg L −1 and 0.03 to 1.58 μg L −1 , respectively. The spiking recoveries of the target analytes were 50.33-127.64% at the levels of 0.2 μg L −1 , 2 μg L −1 and 5 μg L −1 . The precision and accuracy of this method showed a great increase compared with traditional solid-phase extraction. The developed method was successfully applied to extraction and analysis of NSAIDs in different water samples with satisfactory results which could help us better understand their environmental fate and risk to ecological health.
研究领域:
环境科学
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分析化学
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DOI
PubMed
高影响因子
Journal of Functional Foods
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2017
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IF 3.144
Han Peng,Wenting Li,Hongyan Li,Zeyuan Deng,Bing Zhang
Both extractable (EPE) and non-extractable bound phenolic (BPE) in the seed coat and cotyledon of black bean were investigated in the present study. Their total phenolic contents (TPC) and antioxidant activities (DPPH, ABTS and FRAP) were evaluated, and the phytochemical compositions of EPE and BPE in both seed coat and cotyledon of black soybean were identified and quantified ( Glycinemax(L.) merr ) by UPLC-ESI-QTOF-MS/MS and UPLC-ESI-QqQ-MS/MS. In the present study, a total of 112 and 78 compounds were identified or tentatively characterized in the black soybean EPE and BPE, respectively, with the majority being phenolic acids and flavonoids. Seed coat contains more abundant phenolics than that of cotyledon in all fractions. In addition, our results indicated that acid hydrolysis is more thorough than alkaline hydrolysis in the extraction of bound phenolics of black soybean. Our study provides available information for non-extractable bound phenolic constituents and their distribution in the seed coat and cotyledon of black soybean.
研究领域:
植物化学
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食品科学
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DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2022
·
IF 3.571
Baole Zhang,Wanglong Xu,Chuanlong Yin,Yangming Tang
Under the guideline issued by Food and Drug Administration (FDA), ANDAs for Certain Highly Purified Synthetic Peptide Drug Products That Refer to Listed Drugs of rDNA Origin Guidance for Industry , a synthetic Semaglutide that is intended to be a “generic” of the approved rDNA origin Semaglutide is under exploring. Thus, each peptide-related impurity that is 0.10% of the drug substance or greater need to be identified for Semaglutide covered by this guidance. Among others, characterization of the low-level D -amino acid (D form) isomeric impurities are always the most challenging ones. Reverse-phase high-performance liquid chromatography (RP-UPLC) was used to separate the impurities, followed by high resolution mass spectrometry (HRMS) to determine the molecular weight of the impurities that existed in both formulations. Following the targeted D form isomers off-line collection, the samples went through lyophilization, deuterated hydrochloric acid ( D -HCl) hydrolyzation with low level D/L form shifting suppression substrates, chiral derivatization and RP-UPLC tandem mass spectrometry analysis of different amino acids by comparing with standards. Herein, we reported an accurate, straightforward characterization method with low limit of detection for the low-level D -Ser 8 , D -His 1 and D -Asp 9 Semaglutide impurities in Semaglutide formulations. The developed UPLC tandem HRMS method entails a valuable step forward in the detection of trace levels of the D -isomers of Semaglutide and other peptide products.
研究领域:
药学
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分析化学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2019
·
IF 5.399
Fei Xu,Feng Liu,Chaozhan Wang,Yinmao Wei
Magnetic solid-phase extraction (MSPE), using a new reversed-phase/weak anion exchange mix-mode mesoporous magnetic SiO 2 adsorbent, was assessed as an approach for reducing matrix effects in the analysis of six lipophilic marine biotoxins in shellfish using ultrahigh-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The adsorbent showed greater adsorption capacity and selectivity for the analytes and, thus, the MSPE microspheres reduced the matrix effects significantly in the subsequent analysis. In the UPLC-MS/MS analysis, precursor and product ions of the analytes were monitored quantitatively and qualitatively using multiple reaction monitoring and product ion confirmation modes. The proposed method exhibited a linear correlation of 0.9980–0.9991 in the working range for azaspiracids (2.0–200.0 ng/mL) and okadaic acid and its derivatives dinophysistoxins (4.0–200.0 ng/mL) with satisfactory recoveries (82.8–118.6%, RSD < 12%), lower LODs (0.4–1.0 μg/kg) and LOQs (1.0–4.0 μg/kg) than existing methods. In addition, consumption of the adsorbent was reduced, and the MSPE operation is simple and rapid relative to alternatives. These results suggest the proposed method has potential for use in the analysis of lipophilic marine biotoxins in shellfish samples.
研究领域:
分析化学
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海洋生物学
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毒理学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2023
·
IF 3
Chen Yao,Daizhu Lv,Xueqing Zhou,Pengcheng Fu,Wen Sun,Jinlian Chen,Huan Lin
The dynamic modification of RNA plays a crucial role in biological regulation and is strongly linked to human disease development and progression. Notably, modified nucleosides in urine have shown promising potential as early diagnostic biomarkers for various conditions. In this study, we developed and validated a rapid, sensitive, and accurate UPLC-MS/MS method for quantifying eight types of modified nucleosides ( N 1 -methyladenosine (m 1 A), N 6 -methyladenosine (m 6 A), 5-methyluridine (m 5 U), 5-taurinomethyl-2-thiouridine (τm 5 s 2 U), 5-methylcytidine (m 5 C), 2'-O-methylcytidine (Cm), N 1 -methylguanosine (m 1 G), and N 7 -methylguanosine (m 7 G) in human urine. Using the method, we measured the urinary concentrations of m 1 A, m 6 A, m 5 U, τm 5 s 2 U, m 5 C, Cm, m 1 G, and m 7 G in a total of 21 control individuals and 23 patients diagnosed with diabetic retinopathy (DR). Cm levels showed promise as a diagnostic marker for diabetic retinopathy (DR), with a significant value (P < 0.01) and an AUC of 0.735. Other modified nucleosides also exhibited significant differences within specific subpopulations. As non-proliferative diabetic retinopathy (NPDR) signifies the latent early stage of diabetic retinopathy, we developed a multivariate linear model that integrates patients' sex, age, height, and urinary concentration of modified nucleosides which aims to predict and differentiate between healthy individuals, NPDR patients, and proliferative diabetic retinopathy (PDR) patients. Encouragingly, the model achieved satisfactory accuracy rates: healthy (81%), NPDR (75%), and PDR (80%). Our findings provide valuable insights into the development of an early, cost-effective, and noninvasive diagnostic approach for diabetic retinopathy.
研究领域:
医学
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分子生物学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACY AND PHARMACOLOGY
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2023
·Vol. 76
·期 2
·115-121
·
IF 3.3
Ye Zhongjiang,Wang Chenxiang,Li Rongqi,Chen Chuang,Yang Jianhui,Chen Yizhang,Fu Jing,Zhou Tao,Jin Mi,Huang Aifang,Zhang Xiuhua,Zhou Ziye
AimOur study is to investigate the effects of triazole antifungal drugs on the pharmacokinetics of lorlatinib in rats.MethodsThe samples were precipitated with methanol. Chromatographic separation was performed on a ultra-performance liquid chromatography (UPLC) system using a BEH C18 column. The mobile phase consisted of 0.1% formic acid water and methanol. Lorlatinib and crizotinib (internal standard) were detected in multiple reaction monitoring mode. The fragment ions were 407.3–228.07 for lorlatinib and m/z 450.3–260.0 for crizotinib. Lorlatinib and different triazole antifungal drugs were given to Sprague Dawley rats by gavage, and blood was collected from the tail vein at a certain time point. The validated UPLC–MS/MS method was applied to a drug interaction study of ketoconazole, voriconazole, itraconazole, and posaconazole with lorlatinib in rats.ResultsKetoconazole and voriconazole significantly inhibited lorlatinib metabolism. When administration with ketoconazole and voriconazole, the area under the curve from time zero to infinity of lorlatinib increased by 49.0% and 104.3%, respectively; the clearance decreased by 40.0% and 40.0%, respectively. While itraconazole and posaconazole did not affect lorlatinib pharmacokinetics.ConclusionThe UPLC-MS/MS-based assay is helpful to further understand the pharmacokinetics of lorlatinib in rats, and confirmed the findings that the combination of lorlatinib with CYP3A inhibitors should be avoided as predicted by our pre-clinical studies.
研究领域:
药理学
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分析化学
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临床药学
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DOI
PubMed
高影响因子
Analytical Methods
·
2015
·Vol. 8
·期 4
·919-924
·
IF 1.821
Bing Yu,Hailin Cong,Lei Xue,Chao Tian,Xiaodan Xu,Qiaohong Peng,Shujing Yang
Monodisperse silica microspheres with average diameters from 1 μm to 2 μm were synthesized by a modified Stöber method, in which an ethanolic solution of tetraethyl orthosilicate (TEOS) was continuously supplied to the reaction mixture containing KCl electrolyte, water, ethanol and ammonia. The effects of reactant amounts, supply rate, and reaction temperature on the microsphere morphology were investigated. After surface modification with octadecyl trichlorosilane, the obtained monodisperse C18-silica microspheres with an average diameter of 1.5 μm were applied to ultra performance liquid chromatography (UPLC) separation of fullerenes. Because of having a smaller size, the 1.5 μm monodisperse C18-silica UPLC stationary phase shows ultra high efficiency compared with the commercial C18-silica HPLC stationary phase with average diameters from 5 to 50 μm.
研究领域:
材料科学
·
分析化学
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DOI
高影响因子
BMC GASTROENTEROLOGY
·
2025
·Vol. 25
·期 1
·1-17
·
IF 2.6
Lv Jie,Chen Qianqian,Yang Lu,Guan Jing,Wang Sheng,Gui Gen,Yang Zhaoyun,Wang Xu,Sun Bin
IntroductionThe incidence of colorectal cancer (CRC) is increasing with colorectal adenomas recognized as key precancerous lesions. Emerging evidence suggests that Imidazole propionate (ImP), a metabolite of gut microbiota, is elevated in patients, indicating a potential role in tumorigenesis of CRC.ObjectivesThis study aimed to validate a novel method for detecting serum ImP using 3-piperazin-1-yl-propionic acid as an internal standard (IS), and to compare ImP levels between patients with colorectal adenomas and colorectal cancer.Methods Serum ImP were measured using Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry (UPLC-MS/MS) with 3-piperazin-1-yl-propionic acid as the IS. Four distinct patient groups were analyzed.Results The use of 3-piperazin-1-yl-propionic acid as an IS was successfully validated for the quantification of ImP. Serum ImP differed significantly among the groups, showing a stepwise increase from healthy controls to patients with colorectal adenomas and CRC. Notably, ImP concentrations were significantly higher in CRC patients than in other groups.Conclusion This study demonstrates the successful application of 3-piperazin-1-yl-propionic acid as an IS provides a viable method for measuring serum ImP concentrations. The results suggest a potential link between ImP and colorectal cancer development.
研究领域:
医学
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肿瘤学
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微生物组学
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代谢组学
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DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2020
·
IF 3.721
Caiyun Zhang,Jiaxiong Zeng,Wenguang Xiong,Zhenling Zeng
A rapid, simple and reliable method using amoxicillin-D4 as internal standard (IS) for determination of amoxicillin (AMO) in porcine tissues was developed. The analytical methodology used a phosphate buffer (0.01 M, pH = 6.3) with trichloroacetic acid (50 mg/mL) for extraction and Oasis® HLB cartridges for clean-up followed by UPLC-MS/MS analysis. The optimized method was validated according to EU guideline 2002/657/EC and FDA guideline. The LOQ in muscle, fat, liver and kidney were set to 10 μg/kg which was below the maximum residue limits, while the LOD were set to 5 μg/kg. Results showed that using AMO-D4 as IS can effectively eliminate relative matrix interference and improve the recovery and precision. A good linearity was observed at the range of 10−500 μg/kg with a correlation coefficients (R 2 ) larger than 0.99. The mean recoveries were higher than 87.0 %, and the RSDs were lower than 11.2 %. This method could be applied to conveniently analysis the residue of AMO in different porcine tissues.
研究领域:
兽医学
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分析化学
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食品安全
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DOI
高影响因子
危险品化学品经营许可证（带存储）