This paper reported a new analytical method for the simultaneous determination of seven benzotriazole ultraviolet absorbers and seven antibacterial agents in textiles. After ultrasonic extraction for the textile sampl...This paper reported a new analytical method for the simultaneous determination of seven benzotriazole ultraviolet absorbers and seven antibacterial agents in textiles. After ultrasonic extraction for the textile samples in methanol, the solutions were analyzed by ultra-high performance liquid chromotagraphy/orbitrap high resolution mass spectrometry (UPLC/Orbitrap HRMS). It showed that a good chromatographic separation for these target compounds was achieved by a Hypersil GOLD column (100 mm × 2.1 mm × 1.9 μm) with a gradient elution of methanol and 0.1% aqueous formic acid solution (containing 0.5 mmol/L ammonium acetate). Triclosan and 4-chloro-3,5-dimethyl phenol (PCMX) were detected by the orbitrap HRMS in an electrospray ionization (ESI) negative mode while the other twelve target compounds were detected by orbitrap HRMS in ESI positive mode. Full scan experiment was performed over the range from m/z 100 to m/z 500. These target compounds were routinely detected with mass accuracy below 2 × 10-6 (2 ppm) at the optimized conditions. The results showed that the limits of detection (LODs) were in the range from 0.1 to 0.3 μg/kg. The blank samples were spiked at three levels and their average recoveries varied from 80.5% to 96.3% while the relative standard deviation (RSD) changed from 3.2% to 9.9%. The present method was also applied for the determination of those ultraviolet absorbers and antibacterial agents in the commercial textiles.展开更多
This study established a method using gas chromatography-electrostatic field Orbitrap high-resolution mass spectrometry(Orbitrap GC-MS)for the simultaneous determination of 70 organic pollutants across 4 categories:or...This study established a method using gas chromatography-electrostatic field Orbitrap high-resolution mass spectrometry(Orbitrap GC-MS)for the simultaneous determination of 70 organic pollutants across 4 categories:organochlorine pesticides(OCPs),polycyclic aromatic hydrocarbons(PAHs),polychlorinated biphenyls(PCBs),and phthalates(PAEs)in infant cereal-based supplementary foods.Techniques integrating cryogenic centrifugation and lipid and protein adsorbent(LPAS)purification were employed.The precise mass numbers of target compounds were determined by Orbitrap GC-MS in full-scan mode(Full MS),which effectively minimized matrix interferences in these foods.Method validation on rice flour samples demonstrated that the 70 compounds exhibited excellent linearity within their respective mass concentration ranges,with correlation coefficients all exceeding 0.995.The detection limits for this method ranged 0.10–1.00μg/kg,while the quantification limits varied 0.3–3.0μg/kg,meeting the established detection requirements.The average spike recovery of the 70 compounds at 3 spiked levels(5,20,and 100μg/kg)ranged 75.3%–119.3%,with relative standard deviations ranging 1.8%–10.8%.Both inter-day and intra-day precision demonstrated relative standard deviation values below 15%.This method was applied to analyze 100 samples of commercial infant cereal-based supplementary food,revealing the presence of PAEs and PAHs in 12.0%of the samples.Notably,no OCPs or PCBs were detected.The detected concentrations of benzo[a]pyrene(Ba P)and dibutyl phthalate(DBP)were(4.2±0.1)and(1.8±0.3)μg/kg,respectively.This method is straightforward,highly sensitive,and suitable for the rapid screening and confirmation of 70 organic pollutants in infant cereal-based supplementary foods.展开更多
文摘This paper reported a new analytical method for the simultaneous determination of seven benzotriazole ultraviolet absorbers and seven antibacterial agents in textiles. After ultrasonic extraction for the textile samples in methanol, the solutions were analyzed by ultra-high performance liquid chromotagraphy/orbitrap high resolution mass spectrometry (UPLC/Orbitrap HRMS). It showed that a good chromatographic separation for these target compounds was achieved by a Hypersil GOLD column (100 mm × 2.1 mm × 1.9 μm) with a gradient elution of methanol and 0.1% aqueous formic acid solution (containing 0.5 mmol/L ammonium acetate). Triclosan and 4-chloro-3,5-dimethyl phenol (PCMX) were detected by the orbitrap HRMS in an electrospray ionization (ESI) negative mode while the other twelve target compounds were detected by orbitrap HRMS in ESI positive mode. Full scan experiment was performed over the range from m/z 100 to m/z 500. These target compounds were routinely detected with mass accuracy below 2 × 10-6 (2 ppm) at the optimized conditions. The results showed that the limits of detection (LODs) were in the range from 0.1 to 0.3 μg/kg. The blank samples were spiked at three levels and their average recoveries varied from 80.5% to 96.3% while the relative standard deviation (RSD) changed from 3.2% to 9.9%. The present method was also applied for the determination of those ultraviolet absorbers and antibacterial agents in the commercial textiles.
基金funded by National Key Research and Development Program for Young Scientists of China(2022YFF1102900)Hebei Province High-level Talent Funding Project(C20221009)。
文摘This study established a method using gas chromatography-electrostatic field Orbitrap high-resolution mass spectrometry(Orbitrap GC-MS)for the simultaneous determination of 70 organic pollutants across 4 categories:organochlorine pesticides(OCPs),polycyclic aromatic hydrocarbons(PAHs),polychlorinated biphenyls(PCBs),and phthalates(PAEs)in infant cereal-based supplementary foods.Techniques integrating cryogenic centrifugation and lipid and protein adsorbent(LPAS)purification were employed.The precise mass numbers of target compounds were determined by Orbitrap GC-MS in full-scan mode(Full MS),which effectively minimized matrix interferences in these foods.Method validation on rice flour samples demonstrated that the 70 compounds exhibited excellent linearity within their respective mass concentration ranges,with correlation coefficients all exceeding 0.995.The detection limits for this method ranged 0.10–1.00μg/kg,while the quantification limits varied 0.3–3.0μg/kg,meeting the established detection requirements.The average spike recovery of the 70 compounds at 3 spiked levels(5,20,and 100μg/kg)ranged 75.3%–119.3%,with relative standard deviations ranging 1.8%–10.8%.Both inter-day and intra-day precision demonstrated relative standard deviation values below 15%.This method was applied to analyze 100 samples of commercial infant cereal-based supplementary food,revealing the presence of PAEs and PAHs in 12.0%of the samples.Notably,no OCPs or PCBs were detected.The detected concentrations of benzo[a]pyrene(Ba P)and dibutyl phthalate(DBP)were(4.2±0.1)and(1.8±0.3)μg/kg,respectively.This method is straightforward,highly sensitive,and suitable for the rapid screening and confirmation of 70 organic pollutants in infant cereal-based supplementary foods.
文摘基于超高效液相色谱-四极杆静电场轨道阱质谱(UPLC-Q-Exactive Orbitrap-MS)技术及网络药理学探讨化浊散结除痹方治疗痛风性关节炎(gouty arthritis,GA)的药效物质及潜在机制。采用UPLC-Q-Exactive Orbitrap-MS技术鉴定化浊散结除痹方药物成分,对其有效成分进行定性分析,共鉴定出化浊散结除痹方中184个有效成分;通过PharmMapper在线数据库筛选有效成分靶点897个,在OMIM、GeneCards、CTD等数据库获取GA相关的疾病靶点491个,进行韦恩分析后获得二者的交集靶点60个,通过Cytoscape平台构建“成分靶点-GA靶点”网络图,利用STRING数据库构建蛋白-蛋白互作网络,筛选出16个核心靶点,将核心靶点进行基因本体论(Gene Ontology,GO)与京都基因和基因组百科全书(Kyoto Encyclopedia of Genes and Genomes,KEGG)信号通路的富集分析,并构建“成分-靶点-通路”网络图,发现该方治疗GA的主要有效成分为酚类、黄酮类、生物碱类、萜类化合物,关键靶点有SRC、MMP3、MMP9、REN、ALB、IGF1R、PPARG、MAPK1、HPRT1、CASP1,通过GO分析发现其治疗GA主要涉及脂质反应、细菌反应、生物刺激的反应等生物过程,通过KEGG分析发现其治疗GA相关的通路有脂质和动脉粥样硬化、中性粒细胞胞外诱捕网、IL-17等。综上,该研究揭示了酚类、黄酮类、生物碱类、萜类化合物可能是化浊散结除痹方治疗GA的核心药效物质,其药效机制可能与SRC、MMP3、MMP9等靶点及脂质和动脉粥样硬化、中性粒细胞胞外诱捕网、IL-17等通路相关。
