[Objective]The research aimed to establish a liquid chromatography-high-resolution mass spectrometry for detecting residues of diclazuril,toltrazuril and its metabolites in animal-derived food.[Method]The samples were...[Objective]The research aimed to establish a liquid chromatography-high-resolution mass spectrometry for detecting residues of diclazuril,toltrazuril and its metabolites in animal-derived food.[Method]The samples were pre-treated by QuEChERS technology and detected by Exactive liquid chromatography-high resolution mass spectrometry.The liquid chromatography-high-resolution mass spectrometry for detecting the residues of diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide in animal-derived food was established.[Result]Diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide showed a good linear correlation in the range of 2.0-50.0μg/L（r^2〉0.99）.The average recoveries of these four compounds in bovine power at the spiked levels of 2,10 and 20μg/kg were 74.5%-90.1%,and the relative standard deviations（RSD）were 15.4%-17.5%.[Conclusion]This method was stable and reliable,and could be used to detect diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide in animal-derived food.展开更多
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
目的研究清瘟护肺颗粒的化学成分。方法查阅中国知网、PubMed、Web of Science等数据库,检索该制剂组方药材化学成分的相关文献,结合文献报道和ChemicalBook数据库信息,建立化学成分数据库。采用超高效液相色谱-四极杆/静电场轨道阱高...目的研究清瘟护肺颗粒的化学成分。方法查阅中国知网、PubMed、Web of Science等数据库,检索该制剂组方药材化学成分的相关文献,结合文献报道和ChemicalBook数据库信息,建立化学成分数据库。采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLC-Q Exactive Focus MS/MS)法分析制剂的图谱数据,并以Xcalibur 4.0软件拟合分子式,与自建数据库信息进行匹配,初步推测分子式信息,与ChemicalBook或ChemSpider数据库比对,推测化学成分结构。结果共鉴定出158个化学成分,包括苷类36个,黄酮类29个,苯丙素类28个,有机酸类18个,萜类17个,色原酮类8个,其他类22个。结论所建立的方法可系统、准确、快速地定性分析清瘟护肺颗粒中的化学成分。展开更多
基金Supported by Scientific Research Projects of General Administration of Quality Supervision,Inspection and Quarantine“Standard Sample Development and Production System Construction of Animal-derived Veterinary Drugs”(20130143)
文摘[Objective]The research aimed to establish a liquid chromatography-high-resolution mass spectrometry for detecting residues of diclazuril,toltrazuril and its metabolites in animal-derived food.[Method]The samples were pre-treated by QuEChERS technology and detected by Exactive liquid chromatography-high resolution mass spectrometry.The liquid chromatography-high-resolution mass spectrometry for detecting the residues of diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide in animal-derived food was established.[Result]Diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide showed a good linear correlation in the range of 2.0-50.0μg/L（r^2〉0.99）.The average recoveries of these four compounds in bovine power at the spiked levels of 2,10 and 20μg/kg were 74.5%-90.1%,and the relative standard deviations（RSD）were 15.4%-17.5%.[Conclusion]This method was stable and reliable,and could be used to detect diclazuril,toltrazuril,toltrazuril sulfone and toltrazuril sulfoxide in animal-derived food.
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.
