To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry ...To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry （UPLC/MS/MS）. The water samples were extracted and condensed with solid-phase extraction （SPE） using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.展开更多
An environmentally friendly method for extracting sulfonamides（SAs） residues from animal feed was described and applied. The method used online microwave-assisted steam extraction coupled with solid phase extraction...An environmentally friendly method for extracting sulfonamides（SAs） residues from animal feed was described and applied. The method used online microwave-assisted steam extraction coupled with solid phase extraction（MASE-SPE）, which was followed by the analysis using high performance liquid chromatography-mass spectro- metry（HPLC-MS/MS）. The SAs residues were extracted successively with water steam under microwave irradiation, and thus directly introduced into an SPE colunm containing cation-exchange resin. The SAs were then eluted with methanol-ammonia（90：10, volume ratio） from the SPE column and followed by HPLC-MS/IVIS. The limits of detec- tion（LODs） for the analytes ranged from 0.24 ng/g to 0.49 ng/g. The limits of quantification（LOQs） ranged from 0.82 ng/g to 1.63 ng/g. Average recoveries of SAs were 76.3%--92.1%. The developed method was a reliable and envi-ronmentally friendly alternative to previous methods with respect to time, solvent and labor consumption for the analysis of SAs in animal foodstuffs.展开更多
[Objectives]This study was conducted to explore the occurrence levels of endocrine disruptors(EDCs)in rural areas around a county landfill in Tongren City.[Methods]The water around the landfill was sampled and analyze...[Objectives]This study was conducted to explore the occurrence levels of endocrine disruptors(EDCs)in rural areas around a county landfill in Tongren City.[Methods]The water around the landfill was sampled and analyzed.A solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS)method was established for the determination of 27 EDCs.After the HLB solid-phase extraction column was activated,a water sample,which was adjusted with phosphoric acid to a pH of 2(±0.5)and added with 500 mg of disodium EDTA,was loaded,and 5 ml of water and 20%methanol water was added for washing.Next,10 ml of elution solution was added for elution,and the collected eluate was evaporated under reduced pressure at 40℃to near dryness,and 1 ml of reconstitution solution was added to a constant volume.An ACQUITY UPLC BEH C18(100×2.1 mm,2.6μm)chromatographic column was adopted for LC separation by gradient elution with pure water solution-acetonitrile as the mobile phase.For MS detection,the MRM mode was adopted for collection,and the positive and negative ion modes were switched for simultaneous determination,and the internal standard method was used for quantification.[Results]The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance.The limits of quantitation in the method were between 0.05 and 2.00 ng/L,and the recoveries ranged from 75.3%to 105.7%.[Conclusions]The method has high sensitivity,good accuracy and strong practical value.展开更多
基于固相萃取结合超高效液相色谱-串联质谱技术建立同时测定水源水中176种药品和个人护理用品(pharmaceutical and personal care products,PPCPs)含量的方法。将水源水调节至pH 7后,经Cleanert PEP固相萃取柱富集净化,洗脱液采用二甲...基于固相萃取结合超高效液相色谱-串联质谱技术建立同时测定水源水中176种药品和个人护理用品(pharmaceutical and personal care products,PPCPs)含量的方法。将水源水调节至pH 7后,经Cleanert PEP固相萃取柱富集净化,洗脱液采用二甲基亚砜辅助浓缩后,以甲醇-0.1%甲酸水(含0.2 mmol乙酸铵)为流动相,在HSS T3色谱柱(2.1 mm×150 mm,1.8μm)中进行分离,用电喷雾离子源(正负离子切换模式)、多反应监测模式进行测定。方法学验证结果表明,176种PPCPs在5~200 ng/mL范围内线性关系较好,相关系数均高于0.99。176种PPCPs的方法的定量限为0.1 ng/mL。在空白水样中进行3种加标水平(0.1、0.4、1.0 ng/mL)的加标回收实验(n=6),176种化合物的平均回收率在68.0%~126.7%之间,相对标准偏差在1.1%~10.3%之间。综上,本研究所建立的方法简单快速、重现性好、灵敏度高,能够满足水源水中176种PPCPs含量的高通量检测要求。展开更多
基金supported by the Preventive medicine and public health research project of Anhui,China(No.2011Y0103)the Natural Science Foundation of Anhui,China(No.11040606M216)
文摘To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry （UPLC/MS/MS）. The water samples were extracted and condensed with solid-phase extraction （SPE） using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.
基金Supported by the National High Technology Research and Development Program of China（No.2011AA100805） and the National Natural Science Foundation of China（No.20875037）.
文摘An environmentally friendly method for extracting sulfonamides（SAs） residues from animal feed was described and applied. The method used online microwave-assisted steam extraction coupled with solid phase extraction（MASE-SPE）, which was followed by the analysis using high performance liquid chromatography-mass spectro- metry（HPLC-MS/MS）. The SAs residues were extracted successively with water steam under microwave irradiation, and thus directly introduced into an SPE colunm containing cation-exchange resin. The SAs were then eluted with methanol-ammonia（90：10, volume ratio） from the SPE column and followed by HPLC-MS/IVIS. The limits of detec- tion（LODs） for the analytes ranged from 0.24 ng/g to 0.49 ng/g. The limits of quantification（LOQs） ranged from 0.82 ng/g to 1.63 ng/g. Average recoveries of SAs were 76.3%--92.1%. The developed method was a reliable and envi-ronmentally friendly alternative to previous methods with respect to time, solvent and labor consumption for the analysis of SAs in animal foodstuffs.
基金Supported by Tongren Science and Technology Planning Project (TSKY[2022]42)Education Science Planning Project of Department of Education of Guizhou Province (2023B111).
文摘[Objectives]This study was conducted to explore the occurrence levels of endocrine disruptors(EDCs)in rural areas around a county landfill in Tongren City.[Methods]The water around the landfill was sampled and analyzed.A solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS)method was established for the determination of 27 EDCs.After the HLB solid-phase extraction column was activated,a water sample,which was adjusted with phosphoric acid to a pH of 2(±0.5)and added with 500 mg of disodium EDTA,was loaded,and 5 ml of water and 20%methanol water was added for washing.Next,10 ml of elution solution was added for elution,and the collected eluate was evaporated under reduced pressure at 40℃to near dryness,and 1 ml of reconstitution solution was added to a constant volume.An ACQUITY UPLC BEH C18(100×2.1 mm,2.6μm)chromatographic column was adopted for LC separation by gradient elution with pure water solution-acetonitrile as the mobile phase.For MS detection,the MRM mode was adopted for collection,and the positive and negative ion modes were switched for simultaneous determination,and the internal standard method was used for quantification.[Results]The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance.The limits of quantitation in the method were between 0.05 and 2.00 ng/L,and the recoveries ranged from 75.3%to 105.7%.[Conclusions]The method has high sensitivity,good accuracy and strong practical value.
文摘基于固相萃取结合超高效液相色谱-串联质谱技术建立同时测定水源水中176种药品和个人护理用品(pharmaceutical and personal care products,PPCPs)含量的方法。将水源水调节至pH 7后,经Cleanert PEP固相萃取柱富集净化,洗脱液采用二甲基亚砜辅助浓缩后,以甲醇-0.1%甲酸水(含0.2 mmol乙酸铵)为流动相,在HSS T3色谱柱(2.1 mm×150 mm,1.8μm)中进行分离,用电喷雾离子源(正负离子切换模式)、多反应监测模式进行测定。方法学验证结果表明,176种PPCPs在5~200 ng/mL范围内线性关系较好,相关系数均高于0.99。176种PPCPs的方法的定量限为0.1 ng/mL。在空白水样中进行3种加标水平(0.1、0.4、1.0 ng/mL)的加标回收实验(n=6),176种化合物的平均回收率在68.0%~126.7%之间,相对标准偏差在1.1%~10.3%之间。综上,本研究所建立的方法简单快速、重现性好、灵敏度高,能够满足水源水中176种PPCPs含量的高通量检测要求。
