Analytical Methods
·
2022
·Vol. 14
·期 25
·2531-2540
·
IF 3.532
Wenjing Li,Maoyu Cao,Pengxiang Ge,Xiaoyu Fu,Jiajie Tang,Mindong Chen
Organosulfates (OSs) derived from the oxidation of biogenic volatile organic compounds (BVOCs) in the presence of anthropogenic sulfate aerosols are the important tracers of secondary organic aerosols (SOAs). In order to better understand the concentration of pinene-nitrooxy organosulfates (pNOSs) in Nanjing, a sensitive high-performance liquid chromatography-electron spray ionization spectrum/mass spectrum (HPLC-ESI-MS/MS) to determine pNOSs in PM2.5 has been developed and validated in this study. Firstly, Hypersil Gold C18 (Thermo Scientific, San Jose, USA) was selected to separate pinene-derived nitrooxy organosulfates (pNOSs) based on their polarity. Three kinds of pNOSs were detected in the full scan mode (MS) with an ESI source under the negative mode. Secondly, three isomers of pNOSs with fragment ions m/z 220, 151, and 142 were identified based on the MS/MS maps. At least two pairs of transfer ions should be selected as identification and quantification ions according to the optimization results of target compounds. For example, to determine pNOSs, these transfer ions of m/z 294 → 247, m/z 294 → 231, m/z 294 → 220, m/z 294 → 142, m/z 294 → 151, m/z 294 → 96, m/z 294 → 80 were selected as quantification and identification ions. Finally, the influence of scan mode on pNOS detection was evaluated, and the results showed that pNOSs were most sensitive in the SRM (selected reaction monitor) scan mode. Therefore, the SRM scan mode was chosen to detect pNOSs. We applied this method to analyze year-round PM2.5 (PM2.5 is fine particulate matter, which refers to particulate matter in ambient air with an aerodynamic equivalent diameter of less than or equal to 2.5 microns) samples in Nanjing. The average concentration of all the three kinds of pNOSs was 69.95 ng m−3. The results showed that the average concentration of pNOSs was high in spring (92.94 ng m−3) and summer (90.57 ng m−3), and lowest in winter (30.03 ng m−3).
研究领域:
大气化学
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环境科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2021
·Vol. 26
·期 15
·4472
·
IF 4.412
Rurui Li,Yuerong Ru,Zhenxing Wang,Xiahong He,Kin-Weng Kong,Tingting Zheng,Xuechun Zhang
In this study, we aimed to investigate the chemical components and biological activities ofMusella lasiocarpa, a special flower that is edible and has functional properties. The crude methanol extract and its four fractions (petroleum ether, ethyl acetate, n-butanol, and aqueous fractions) were tested for their total antioxidant capacity, followed by their α-glucosidase, acetylcholinesterase, and xanthine oxidase inhibitory activities. Among the samples, the highest total phenolic and total flavonoid contents were found in the ethyl acetate (EtOAc) fraction (224.99 mg GAE/g DE) and crude methanol extract (187.81 mg QE/g DE), respectively. The EtOAc fraction ofMusella lasiocarpaexhibited the strongest DPPH· scavenging ability, ABTS·+scavenging ability, and α-glucosidase inhibitory activity with the IC50values of 22.17, 12.10, and 125.66 μg/mL, respectively. The EtOAc fraction also showed the strongest ferric reducing antioxidant power (1513.89 mg FeSO4/g DE) and oxygen radical absorbance capacity ability (524.11 mg Trolox/g DE), which were higher than those of the control BHT. In contrast, the aqueous fraction demonstrated the highest acetylcholinesterase inhibitory activity (IC50= 10.11 μg/mL), and the best xanthine oxidase inhibitory ability (IC50= 5.23 μg/mL) was observed from the crude methanol extract as compared with allopurinol (24.85 μg/mL). The HPLC-MS/MS and GC-MS analyses further revealed an impressive arsenal of compounds, including phenolic acids, fatty acids, esters, terpenoids, and flavonoids, in the most biologically active EtOAc fraction. Taken together, this is the first report indicating the potential ofMusella lasiocarpaas an excellent natural source of antioxidants with possible therapeutic, nutraceutical, and functional food applications.Keywords:Musella lasiocarpa;antioxidant activity;α-glucosidase;xanthine oxidase;acetylcholinesterase;HPLC-MS/MS;GC-MS
研究领域:
植物化学
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药理学
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营养学
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DOI
PubMed
高影响因子
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2020
·Vol. 34
·期 10
·e8742
·
IF 2.2
Jichao Liu,Guoliang Li,Di Wu,Yanxin Yu,Jian Chen,Yongning Wu
Rationale Sedatives, which are prone to cause residues in animals, have been abused in modern animal husbandry. Long-term consumption of contaminated meat products would be unfavorable to the human nervous system. Taking into account public health and food safety, it was essential to develop an effective method for the enrichment and detection of sedatives in meat. Methods Fe 3 O 4 @TbBd@ZIF-8 composites were synthesized by using Fe 3 O 4 nanoparticles as a magnetic core and 1,3,5-triformylbenzene (Tb) and benzidine (Bd) as two building blocks to form Fe 3 O 4 @TbBd. Furthermore, the zeolitic imidazolate framework-8 (ZIF-8) was modified on the surface of the Fe 3 O 4 @TbBd. In addition, Fe 3 O 4 @TbBd@ZIF-8 was used as a magnetic solid-phase extraction (MSPE) adsorbent of typical animal sedatives in pork samples. Mass spectrometry analysis was conducted by electrospray ionization triple-quadrupole mass spectrometry in positive-ion multiple reaction monitoring mode. Results By combining the optimized MSPE approach with high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS), an accurate and sensitive method for the determination of sedatives was developed. The method exhibited good linearity in the range of 0.03–70 μg/kg with the correlation coefficient (R 2 ) ranging from 0.9982 to 0.9999, high sensitivity with limits of detection (LODs) ranging from 0.04 to 0.2 μg/kg, and high precision with relative standard deviation (RSD) less than 5.5%. The adsorption behaviors of Fe 3 O 4 @TbBd@ZIF-8 towards sedatives were more suitably described by a pseudo-second-order kinetic and Freundlich isotherm model. Conclusions The proposed MSPE-HPLC/MS/MS method was successfully applied to the determination of sedatives in real samples and showed excellent applicability. Several sedatives were detected in the selected meat samples. The developed method was shown to be facile, sensitive and accurate for sedative detection and also showed great prospects for determination of sedatives from other complex samples.
研究领域:
分析化学
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食品安全
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材料科学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Cheng Xin,Jingming Zhou,Yumei Chen,Yankai Liu,Hongliang Liu,Chao Liang,Xifang Zhu,Ying Zhang,Zhuting Chen,Xueyuan Tang,Bingxue Zhang,Mengjun Lu,Jiaojiao Wei,Hua Xue,Yanhua Qi,Gaiping Zhang,Aiping Wang
Florfenicol (F), an antimicrobial agent exclusive to veterinary use within the chloramphenicol class, is extensively applied as a broad-spectrum remedy for animal diseases. Despite its efficacy, concerns arise over potential deleterious residues in animal-derived edibles, posing threats to human health. This study pioneers an innovative approach, introducing a quantum dot fluorescence-based immunoassay (FLISA) for the meticulous detection of F residues in animal-derived foods and feeds. This method demonstrates heightened sensitivity, with a detection limit of 0.3 ng/mL and a quantitative detection range of 0.6–30.4 ng/mL. Method validation, applied to diverse food sources, yields recoveries from 90.4 % to 109.7 %, featuring RSDs within 1.3 % to 8.7 %, the results showed high consistency with the national standard HPLC-MS/MS detection method. These findings underscore the method's accuracy and precision, positioning it as a promising tool for swift and reliable F residue detection, with substantial implications for fortifying food safety monitoring.
研究领域:
兽医学
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食品安全
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分析化学
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生物技术
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产品关联
DOI
PubMed
高影响因子
Scientific Reports
·
2025
·Vol. 15
·期 1
·1-8
·
IF 3.9
Wang Yueyuan,Diao Zhipeng,Qu Yuchen,Fan Kai,Feng Chen,Lv Bo,Yu Yunli,Geng Zhou
Omadacycline, a third-generation tetracycline antibiotic, exhibits time-dependent pharmacokinetics. The ratio of the 24-hour area under the concentration-time curve to minimum inhibitory concentration (AUC 0−24 /MIC) serves as the primary pharmacokinetic/pharmacodynamic (PK/PD) index for omadacycline, demonstrating strong correlation with therapeutic efficacy, particularly in critically ill patient populations. To facilitate routine therapeutic drug monitoring (TDM) in clinical practice, a high-performance liquid chromatography - tandem mass spectrometry (HPLC-MS/MS) method was developed for quantification of omadacycline in human plasma. An Agilent 1260 series liquid chromatograph and an API 4000 triple tandem quadrupole mass spectrometer were used for the determination of omadacycline and endocannabinoids. The separation was performed on a Phenomenex KINETEX XB-C18 column (2.6 μm, 3 × 50 mm) with 0.1% formic acid-water and pure acetonitrile as the mobile phases. The LC-MS/MS separation was carried out using a gradient elution procedure at a flow rate of 0.4 mL/ min, and the total run time was 5 min. An electrospray ionization (ESI) was selected, and the detection ions of omadacycline and the internal standard (fexofenadine-d6) were determined by mass spectrometry scanning with multiple reaction monitoring (MRM) in positive ion mode as follows: m/z 557.4→453.4 and m/z 508.4→472.8, respectively. The established linear range (20-2000 ng/mL) effectively covers the plasma concentration range encountered in > 98% of clinical samples, making it suitable for routine therapeutic drug monitoring. The method demonstrated acceptable selectivity, recovery, and matrix effect. The results of intra-day precision and inter-day precision show that the relative standard deviation (RSD) is less than 10%, while the relative error (RE) is within ± 10.00%. In this study, we developed and validated a simple, sensitive and accurate method to quantify the concentration of omadacycline in human plasma using LC-MS/MS. This offers essential technical support for the rational clinical application of omadacycline.
研究领域:
药理学
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分析化学
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临床药理学
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质谱分析
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治疗药物监测
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DOI
PubMed
高影响因子
Foods
·
2023
·Vol. 12
·期 24
·4476
·
IF 5.2
Yujiao Zhang,Haoran Song,Zhengqi Liu,Chunqing Ai,Chunhong Yan,Xiuping Dong,Shuang Song
Due to its significant physiological effects, a sulfated polysaccharide has been considered an important nutrient of sea cucumber, but its metabolism in vivo is still unclear. The present study investigated the metabolism of a sea cucumber sulfated polysaccharide (SCSP) in rats and its influence on the metabolite profiles. The quantification by HPLC-MS/MS revealed that the blood level of SCSP achieved a maximum of 54.0 ± 4.8 μg/mL at 2 h after gavage, almost no SCSP was excreted through urine, and 55.4 ± 29.8% of SCSP was eliminated through feces within 24 h. These results prove the utilization of SCSP by gut microbiota, and a further microbiota sequencing analysis indicated that the SCSP utilization in the gut was positively correlated with Muribaculaceae and Clostridia_UCG-014. In addition, the non-targeted metabolomic analysis demonstrated the significant effects of SCSP administration on the metabolite profiles of blood, urine, and feces. It is worth noting that the SCSP supplement decreased palmitic acid, stearic acid, and oleic acid in blood and urine while increasing stearic acid, linoleic acid, and γ-linolenic acid in feces, suggesting the inhibition of fat absorption and the enhancement of fat excretion by SCSP, respectively. The present study shed light on the metabolism in vivo and the influence on the fat metabolism of SCSP.Keywords:marine polysaccharides;intestinal flora;nontargeted metabolomics
研究领域:
海洋生物学
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营养学
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微生物学
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代谢组学
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产品关联
DOI
PubMed
高影响因子
GLYCOCONJUGATE JOURNAL
·
2017
·Vol. 34
·期 5
·625-632
·
IF 2.186
Song Shuang,Yu Qi,Zhang Bao,Ai Chunqing,Sun Yujiao,Fu Yinghuan,Zhao Meiyu,Wen Chengrong
Fish intestines and livers are usually considered as delicious and nutritious food in China. Acidic polysaccharides are important nutrients in these food of animal origin, but there is currently little information regarding their quantitative distributions. The present study demonstrated a method to quantify acidic polysaccharides simultaneously by analyzing their disaccharides produced from the acid hydrolysis using high-performance liquid chromatography (HPLC) coupled with triple quadrupole mass spectrometry. The recoveries for these acidic polysaccharides were all 97%–115% with relative standard deviation of 3.0%–9.0%. All of the acidic polysaccharides had good linearities. Then this method was applied to determine the composition of acidic polysaccharides in 5 edible fish livers and intestines. Besides well-known glycosaminoglycans (GAGs) including hyaluronic acid (HA), Chondroitin sulfate (CS), dermatan sulfate (DS) and heparin (HP), 4 novel acidic polysaccharides including 2 GAGs and 2 non-GAGs comprised of hexose-hexuronic acid repeating units were also found. CS and HP were the major acidic polysaccharides components in fish intestines and livers, respectively. The absolute amounts of acidic polysaccharides differed greatly in these fish tissues, but their proportions showed similarity in the same type of tissues. The present study demonstrated an effective method for acidic polysaccharides quantification, and revealed acidic polysaccharides compositions of edible fish livers and intestines.
研究领域:
食品科学
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分析化学
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营养学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2025
·
IF 3.8
Xu Jiaqi,Li Qianyu,Li Wenrui,Wu Di,Wu Yongning,Li Guoliang
Matrix effects pose a significant challenge in food analysis for the quantitative analysis of complex food samples. Herein, a novel magnetic covalent organic framework nanocomposite and the copper(I)-catalyzed azide–alkyne cycloaddition (CuAAC) click reaction-based stable isotope labeling (SIL) method were presented for highly selective and sensitive detection of steroid hormones in food samples using HPLC-MS/MS. The nanocomposite, Fe 3 O 4 @TAPB-COF, with a core–shell structure exhibited high adsorption capacities for steroid hormones. Combined with a SIL method based on the CuAAC click reaction, steroid hormones were accurately quantified in food samples with high sensitivity and selectivity. A pair of SIL agents, N -(2-azidoethyl)aniline (d 0 -NAEA) and d 5 - N -(2-azidoethyl)aniline (d 5 -NAEA), was synthesized to label steroid hormones in the samples and standard solutions, respectively. The labeling reaction is highly specific, and the formation of the derivatives is easily ionized by MS, thus overcoming matrix effects. More surprisingly, the ionization efficiency of steroid hormones increased by a factor of 4 to 56, with matrix effects ranging from 87.3 to 99.3%. Under optimal conditions, this method exhibited a low limit of detection (LOD) ranging from 0.1 to 2.6 μg L −1 and overcame the interference of matrix effects for trace-level steroid hormone analysis in foodstuffs.
研究领域:
分析化学
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食品安全
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生物医学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2014
·
IF 2.694
Xin Liu,Yuan Hong,Qing He,Kai Huang
A simple, rapid and sensitive high-performance liquid chromatography–tandem mass spectrometric (HPLC–MS/MS) method was developed and validated for determining lycorine in rat plasma. Plasma samples were prepared by a simple protein precipitation with methanol containing dextrorphan as internal standard. The chromatographic separation was performed on a Kromasil 60-5CN column (3 μm, 2.1 mm × 150 mm) with the mobile phase of methanol/water (containing 0.1% formic acid) (40:60, v/v) at a flow rate of 0.2 mL/min, the total analytical runtime was 5 min. The detection was performed on a triple quadrupole tandem mass spectrometer equipped with Electronic Spray Ion by selected reaction monitoring (SRM) of the transitions at m / z 288.1 → 147.1 for lycorine and m / z 258.1 → 157.2 for dextrorphan, respectively. The calibration curve was linear over the range of 1–1000 ng/mL with the lower limit of quantification of 1 ng/mL for lycorine. The intra- and inter-day precision (R.S.D.%) were less than 8.5% and accuracy (R.E.%) was within ±7.0%. Lycorine was sufficiently stable under all relevant analytical conditions. This method was successfully applied to the pharmacokinetic study of lycorine in rats after intraperitoneal administration with different doses of 5, 10 and 20 mg/kg.
研究领域:
分析化学
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药物代谢动力学
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毒理学
✓ 已验证
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2026
·
IF 3.4
Cui’e Qi,Jiaqi Song,Longwei Lv,Yidi Yin,Siyao Wang,Meng Li,Qing Li
A robust HPLC method employing a polysaccharide-based chiral stationary phase was developed and optimized for the enantiomeric separation of tetrahydrojatrorrhizine. Investigations into the effects of chromatographic conditions on enantiomeric separation revealed that a specific mobile phase, comprising methanol and ammonium acetate solution, significantly enhanced enantioselectivity with a resolution of 1.89 at a lower column temperature. Thermodynamic analysis based on van’t Hoff plots was carried out, which demonstrated a clear enthalpy-driven potential for chiral recognition, suggesting binding interactions played the dominant role in enantiomeric separation. To elucidate molecular mechanisms of chiral recognition, the complementary docking simulation was also performed, identifying that the observed enantioselectivity originated from differences in the key interactions, including hydrogen bond, π-π stacking, and steric hindrance. Additionally, a chiral HPLC-MS/MS method was fully validated for the determination of tetrahydrojatrorrhizine enantiomers in rat plasma, and applied to a preliminary enantioselective pharmacokinetic study. The results showed significantly different pharmacokinetic profiles between the two enantiomers, highlighting that the area under the curve of S -(−)-tetrahydrojatrorrhizine was statistically higher than that of R -(+)-tetrahydrojatrorrhizine. The integrated work presented herein provided a reliable analytical method and mechanistic insights into chiral recognition of tetrahydrojatrorrhizine enantiomers, supporting the precise evaluation of enantiomeric behaviors in vivo .
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DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2024
·
IF 5.7
Linbin Zheng,Meng Li,Zhouyu Jiang,Junyan Fan,Zengbo Fang,Jihuai Zheng,Yan Cui
Background The increased production and use of chiral pesticides will enhance their exposure in the environment. Chiral pesticides typically exhibit varied biological effects among these enantiomers. Therefore, it is very essential to develop and validate chiral analytical methods to investigate their potential ecological risks from a stereoselective perspective. Current separation of pesticides enantiomers relies extensively on chiral stationary phases (CSPs), while the development of β-Cyclodextrin derivatives CSPs become the research focus due to their great modifiability and excellent chiral recognition capabilities. Results A novel chiral stationary phase, 3,5-dichlorophenylaminomethyl-6-phenylenediamine-β-cyclodextrin chemically bonded silica gel (MPDCDA), was successfully prepared. Based on that, a stereoselective HPLC-MS/MS method was developed and validated for the determination of tebuconazole enantiomers in Rana nigromaculata tadpoles. After extraction by QuEChERS, the tebuconazole enantiomers were completely separated with the resolutions of 1.63 using the mobile phase of methanol-water (70/30, v/v). Good linearity (r > 0.9990) for both enantiomers over a concentration range of 0.20–500.0 ng/mL was obtained with the accuracy ranged from 6.7 % to 9.3 % and the intra-day and inter-day precisions below 6.2 % at three quality control levels. The proposed method was successfully applied in evaluating the enantioselective bioaccumulation and elimination profiles of tebuconazole in tadpoles. At the tested conditions, there was no significantly enantioselective difference in the bioaccumulation process for S - tebuconazole and R -tebuconazole. However, the elimination process of tebuconazole enantiomers was enantioselective with R -tebuconazole preferentially degraded. Significance This work provided an accurate risk assessment of chiral pesticides to non-target aquatic organisms from a stereoselective perspective. These findings would deepen our understanding of the potential ecological risks of chiral pesticides on aquatic organisms and provide scientific support for the protection of aquatic organisms and their ecological environments, as well as sustainable development.
研究领域:
分析化学
·
环境科学
·
生态毒理学
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产品关联
DOI
PubMed
高影响因子
TALANTA
·
2017
·
IF 4.162
Xiu-Xiu Dong,Li-Peng Yuan,Yi-Xin Liu,Min-Fu Wu,Bo Liu,Yuan-Ming Sun,Yu-Dong Shen,Zhen-Lin Xu
Progesterone (P4) is a kind of hormone that can cause neuropathic disturbances in humans when the concentration overpasses a certain degree. In this work, an electrochemical immunosensor capable of detecting P4 sensitively and selectively was developed. Thionine-graphene oxide (Thi-GO) composites with excellent biocompatibility were synthesized and coated to a clear glassy carbon electrode. P4 coating antigen (P4-OVA) was immobilized to the electrode, then sample as well as biotinylated antibody (biotin-P4 Ab) were added. The free P4 can compete with P4-OVA for binding to biotin-P4 Ab. After the further addition of streptavidin-HRP, H 2 O 2 was introduced to develop electrical signal for quantitative determination of P4. After careful optimization of assay conditions, the proposed immunosensor showed a linear range from 0.02 to 20ngmL −1 for P4 in milk samples. The averaged recoveries from spiked samples ranged from 84.0% to 102.0%, which correlated well with standard HPLC-MS/MS. The biosensor also showed good specificity, reproducibility and stability, indicating its potential application in monitoring of P4 in a simple and low cost manner.
研究领域:
分析化学
·
生物传感器
·
电化学
·
纳米材料
✓ 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）