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
目的通过超高效液相色谱—质谱联用(ultra-performance liquid chromatography-orbitrap-mass spectrometry/mass spectrometry,UPLC-Orbitrap-MS/MS)对通络益晴方的化学成分进行快速分析及初步鉴定。方法使用ZORBAX Eclipse Plus C 18...目的通过超高效液相色谱—质谱联用(ultra-performance liquid chromatography-orbitrap-mass spectrometry/mass spectrometry,UPLC-Orbitrap-MS/MS)对通络益晴方的化学成分进行快速分析及初步鉴定。方法使用ZORBAX Eclipse Plus C 18色谱柱,以乙腈-0.1%甲酸水梯度洗脱,流速0.4 mL/min,柱温35℃;采用电喷雾离子源,正、负离子模式扫描,通过保留时间、精确相对分子质量和二级质谱裂解碎片,结合参考文献,对所得成分进行分析与初步鉴定。结果根据建立的色谱条件,从通络益晴方中初步鉴定出94个化学成分,其中有黄酮类化合物31个、酚酸类化合物14个、脂肪酸类化合物9个、皂苷类化合物6个、异黄酮类化合物5个、氨基酸类化合物4个、三萜类化合物4个、醛类化合物4个、多肽类化合物3个、苯丙素类化合物3个、醇类化合物3个,以及其他类化合物8个;正、负离子扫描模式下得到8个重复的成分。结论UPLC-Orbitrap-MS/MS技术能快速、初步鉴定出通络益晴方中化学成分,可为通络益晴方物质基础研究和新药研发提供依据。展开更多
To effectively assess the extent of the mycotoxin contamination of grapes,a method was developed to analyze 22 mycotoxins by ultra-high-performance liquid chromatography coupled with quadrupole/orbitrap high-resolutio...To effectively assess the extent of the mycotoxin contamination of grapes,a method was developed to analyze 22 mycotoxins by ultra-high-performance liquid chromatography coupled with quadrupole/orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS).Samples were extracted and purified using the QuEChERS(quick,easy,cheap,effective,rugged,and safe)procedure.The extracts were separated on a BEH Shield C18 column(100 mm×2.1 mm,1.7μm),using methanol and water with 0.1%formic acid solution and 2 mmol/L ammonium acetate as the mobile phases.The quantification was performed according to a matrix-matched external standard method.There was a good linear relationship within the respective mass concentration ranges of 22 mycotoxins;the correlation coefficients were not less than 0.9981.The limit of quantification was 0.3-10.0μg/kg.Mycotoxin recovery ranged from 68.6%to 109.0%,with a relative standard deviation of 1.28%-12.80%.The method is simple,rapid,highly sensitive,and accurate,making it useful for screening grapes for common and emerging mycotoxins.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.
文摘目的通过超高效液相色谱—质谱联用(ultra-performance liquid chromatography-orbitrap-mass spectrometry/mass spectrometry,UPLC-Orbitrap-MS/MS)对通络益晴方的化学成分进行快速分析及初步鉴定。方法使用ZORBAX Eclipse Plus C 18色谱柱,以乙腈-0.1%甲酸水梯度洗脱,流速0.4 mL/min,柱温35℃;采用电喷雾离子源,正、负离子模式扫描,通过保留时间、精确相对分子质量和二级质谱裂解碎片,结合参考文献,对所得成分进行分析与初步鉴定。结果根据建立的色谱条件,从通络益晴方中初步鉴定出94个化学成分,其中有黄酮类化合物31个、酚酸类化合物14个、脂肪酸类化合物9个、皂苷类化合物6个、异黄酮类化合物5个、氨基酸类化合物4个、三萜类化合物4个、醛类化合物4个、多肽类化合物3个、苯丙素类化合物3个、醇类化合物3个,以及其他类化合物8个;正、负离子扫描模式下得到8个重复的成分。结论UPLC-Orbitrap-MS/MS技术能快速、初步鉴定出通络益晴方中化学成分,可为通络益晴方物质基础研究和新药研发提供依据。
基金supported by Science and Technology Program of the State Administration for Market Regulation of China (2020MK014).
文摘To effectively assess the extent of the mycotoxin contamination of grapes,a method was developed to analyze 22 mycotoxins by ultra-high-performance liquid chromatography coupled with quadrupole/orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS).Samples were extracted and purified using the QuEChERS(quick,easy,cheap,effective,rugged,and safe)procedure.The extracts were separated on a BEH Shield C18 column(100 mm×2.1 mm,1.7μm),using methanol and water with 0.1%formic acid solution and 2 mmol/L ammonium acetate as the mobile phases.The quantification was performed according to a matrix-matched external standard method.There was a good linear relationship within the respective mass concentration ranges of 22 mycotoxins;the correlation coefficients were not less than 0.9981.The limit of quantification was 0.3-10.0μg/kg.Mycotoxin recovery ranged from 68.6%to 109.0%,with a relative standard deviation of 1.28%-12.80%.The method is simple,rapid,highly sensitive,and accurate,making it useful for screening grapes for common and emerging mycotoxins.
