Objective To establish a comprehensive analytical method based on SPE‐UPLC‐MS for the simultaneous determination of bisphenol A （BPA）, nonylphenol （NP）, and octylphenol （OP） in urine samples. Methods Sixty uri...Objective To establish a comprehensive analytical method based on SPE‐UPLC‐MS for the simultaneous determination of bisphenol A （BPA）, nonylphenol （NP）, and octylphenol （OP） in urine samples. Methods Sixty urine samples collected from healthy subjects were analyzed for BPA, NP, and OP concentrations. The samples were de‐conjugated by adding β‐glucuronidase and sulfatase. After the enzymatic treatment, the samples were subjected to the OASIS HLB column solid phase extraction cartridges so as to be cleaned and concentrated. The UPLC separation was performed on a Acquity UPLCTM BEH C18 column （2.1×100 mm, 1.7 μm） with a gradient elution system of methanol‐water as the mobile phase. Triple‐quadrupole mass spectrometry analyzer was used for the qualitative and quantitative analysis of UPLC‐MS/MS system. Results The limit of detection of BPA, NP, and OP was 0.10, 0.10, and 0.15 ng/mL, respectively. The recoveries of BPA, NP and OP were 80.1%‐108%, 81.3%‐109%, and 81.5%‐98.7%, respectively. Among the 60 urine samples, BPA was detected in 8 samples at the level of 0.297‐32.7ng/mL, NP was detected in 29 samples at the level of 1.69‐27.8 ng/mL, and OP was detected in 17 samples at the level of 0.407‐11.1 ng/mL. Conclusion The method is simple with high sensitivity and selectivity, and is suitable for the determination of BPA, NP, and OP in urine. As shown by our analysis , BPA, NP, and OP appear to be prevalent in human urine. This is particularly true for NP. The results from our study is therefore valuable for future studies to assess the exposure to BPA, NP, and OP in the general population.展开更多
潜蝇姬小蜂属Diglyphus寄生蜂是潜叶蝇类害虫的重要天敌。本文对其种类、分布、田间发生和优势度、优势种的控害特性和生态适应性,以及优势种的人工繁殖和田间应用等进行总结和展望,以期为更好地应用该属寄生蜂防控我国潜叶蝇的研究和...潜蝇姬小蜂属Diglyphus寄生蜂是潜叶蝇类害虫的重要天敌。本文对其种类、分布、田间发生和优势度、优势种的控害特性和生态适应性,以及优势种的人工繁殖和田间应用等进行总结和展望,以期为更好地应用该属寄生蜂防控我国潜叶蝇的研究和应用提供指导。迄今已鉴定该属寄生蜂36种,全为抑性外寄生蜂,其中针对豌豆潜蝇姬小蜂D.isaea、贝氏潜蝇姬小蜂D.begini和中带潜蝇姬小蜂D.intermedius的研究较多。雌蜂不仅可通过繁殖型的寄生方式而且还可通过非繁殖型方式(取食寄主和产卵器插入直接杀死)致死寄主。雌蜂偏好寄生大个体寄主和取食相对较小个体的寄主,且雌蜂对寄主幼虫的偏好具有"寄主大小依赖型性别分配"现象(host-size-dependent sex allocation)。从温度适应范围和控害潜力首推为豌豆潜蝇姬小蜂。优势种的规模饲养技术已经被研发并得到了较广泛的田间应用。未来研究可主要集中于:(1)加强优势种尤其是温度适应范围广或较为耐热的种群或地理品系的研究,以增加对三叶草斑潜蝇Liriomyza trifolii和美洲斑潜蝇L.sativae的控效;(2)加强雌蜂寄主取食行为特性及其生理机制的研究,以更高效利用;(3)因地制宜研发规模化饲养技术和释放技术;(4)加强潜蝇姬小蜂同其他潜叶蝇寄生蜂的协同控害及竞争共存机制的研究,已提升对潜叶蝇的生防控制效果。展开更多
Xiao-Xu-Ming decoction（XXMD） was a traditional Chinese prescription and first recorded in ＂Bei Ji Qian Jin Yao Fang＂.It has been widely used to treat theoplegia and the sequel of theoplegia in China.In the present...Xiao-Xu-Ming decoction（XXMD） was a traditional Chinese prescription and first recorded in ＂Bei Ji Qian Jin Yao Fang＂.It has been widely used to treat theoplegia and the sequel of theoplegia in China.In the present work,high-performance liquid chromatography coupled with high resolution mass spectrometry（HPLC-HRMS） combined with the mass spectral tree similarity filter technique（MTSF）was used to rapidly discover and identify the compounds of the active fraction of XXMD.A total of 3362 compounds were automatically detected by HPLC-HRMS,and final 68 compounds were identified in the active fraction of XXMD.including 14 templated compounds（reference compounds）,50 related compounds fished by MTSF technique,and 4 unrelated compounds identified by manual method.This study successfully applied MTSF technology for the first time to discover and identify the components of Chinese prescription.The results demonstrated that MTSF technique should be useful to the discovery and identification of compounds in Chinese prescription.This study also proved that MTSF can be applied to the targeted phytochemical separation.展开更多
Accurate mass measurements of 20 drugs were conducted using MassWorks software on a TSQ Quantum Ultra mass spectrometer. All Q1 scan mass spectral data were collected in profile mode with full width at half-maximum（F...Accurate mass measurements of 20 drugs were conducted using MassWorks software on a TSQ Quantum Ultra mass spectrometer. All Q1 scan mass spectral data were collected in profile mode with full width at half-maximum（FWHM） set at 0.7 Da.The mass errors of all 20 drugs（molecular weight between 135 and 810） were within the range from-22.4×10-6 to 36.1×10-6,among them 90% of the drugs achieved a mass accuracy better than 10×10-6.The new method can provide accurate mass measurements on unit mass resolution mass spectrometers.展开更多
基金supported by the National Science and Technology Fundation as par of the Key Technologies of Food Safety Project. Chemical pollutants exposure assessment technology research(2006BAK02A01)
文摘Objective To establish a comprehensive analytical method based on SPE‐UPLC‐MS for the simultaneous determination of bisphenol A （BPA）, nonylphenol （NP）, and octylphenol （OP） in urine samples. Methods Sixty urine samples collected from healthy subjects were analyzed for BPA, NP, and OP concentrations. The samples were de‐conjugated by adding β‐glucuronidase and sulfatase. After the enzymatic treatment, the samples were subjected to the OASIS HLB column solid phase extraction cartridges so as to be cleaned and concentrated. The UPLC separation was performed on a Acquity UPLCTM BEH C18 column （2.1×100 mm, 1.7 μm） with a gradient elution system of methanol‐water as the mobile phase. Triple‐quadrupole mass spectrometry analyzer was used for the qualitative and quantitative analysis of UPLC‐MS/MS system. Results The limit of detection of BPA, NP, and OP was 0.10, 0.10, and 0.15 ng/mL, respectively. The recoveries of BPA, NP and OP were 80.1%‐108%, 81.3%‐109%, and 81.5%‐98.7%, respectively. Among the 60 urine samples, BPA was detected in 8 samples at the level of 0.297‐32.7ng/mL, NP was detected in 29 samples at the level of 1.69‐27.8 ng/mL, and OP was detected in 17 samples at the level of 0.407‐11.1 ng/mL. Conclusion The method is simple with high sensitivity and selectivity, and is suitable for the determination of BPA, NP, and OP in urine. As shown by our analysis , BPA, NP, and OP appear to be prevalent in human urine. This is particularly true for NP. The results from our study is therefore valuable for future studies to assess the exposure to BPA, NP, and OP in the general population.
文摘潜蝇姬小蜂属Diglyphus寄生蜂是潜叶蝇类害虫的重要天敌。本文对其种类、分布、田间发生和优势度、优势种的控害特性和生态适应性,以及优势种的人工繁殖和田间应用等进行总结和展望,以期为更好地应用该属寄生蜂防控我国潜叶蝇的研究和应用提供指导。迄今已鉴定该属寄生蜂36种,全为抑性外寄生蜂,其中针对豌豆潜蝇姬小蜂D.isaea、贝氏潜蝇姬小蜂D.begini和中带潜蝇姬小蜂D.intermedius的研究较多。雌蜂不仅可通过繁殖型的寄生方式而且还可通过非繁殖型方式(取食寄主和产卵器插入直接杀死)致死寄主。雌蜂偏好寄生大个体寄主和取食相对较小个体的寄主,且雌蜂对寄主幼虫的偏好具有"寄主大小依赖型性别分配"现象(host-size-dependent sex allocation)。从温度适应范围和控害潜力首推为豌豆潜蝇姬小蜂。优势种的规模饲养技术已经被研发并得到了较广泛的田间应用。未来研究可主要集中于:(1)加强优势种尤其是温度适应范围广或较为耐热的种群或地理品系的研究,以增加对三叶草斑潜蝇Liriomyza trifolii和美洲斑潜蝇L.sativae的控效;(2)加强雌蜂寄主取食行为特性及其生理机制的研究,以更高效利用;(3)因地制宜研发规模化饲养技术和释放技术;(4)加强潜蝇姬小蜂同其他潜叶蝇寄生蜂的协同控害及竞争共存机制的研究,已提升对潜叶蝇的生防控制效果。
基金the Natural Science Foundation of Beijing(No.7133252) for financial support of this work
文摘Xiao-Xu-Ming decoction（XXMD） was a traditional Chinese prescription and first recorded in ＂Bei Ji Qian Jin Yao Fang＂.It has been widely used to treat theoplegia and the sequel of theoplegia in China.In the present work,high-performance liquid chromatography coupled with high resolution mass spectrometry（HPLC-HRMS） combined with the mass spectral tree similarity filter technique（MTSF）was used to rapidly discover and identify the compounds of the active fraction of XXMD.A total of 3362 compounds were automatically detected by HPLC-HRMS,and final 68 compounds were identified in the active fraction of XXMD.including 14 templated compounds（reference compounds）,50 related compounds fished by MTSF technique,and 4 unrelated compounds identified by manual method.This study successfully applied MTSF technology for the first time to discover and identify the components of Chinese prescription.The results demonstrated that MTSF technique should be useful to the discovery and identification of compounds in Chinese prescription.This study also proved that MTSF can be applied to the targeted phytochemical separation.
文摘Accurate mass measurements of 20 drugs were conducted using MassWorks software on a TSQ Quantum Ultra mass spectrometer. All Q1 scan mass spectral data were collected in profile mode with full width at half-maximum（FWHM） set at 0.7 Da.The mass errors of all 20 drugs（molecular weight between 135 and 810） were within the range from-22.4×10-6 to 36.1×10-6,among them 90% of the drugs achieved a mass accuracy better than 10×10-6.The new method can provide accurate mass measurements on unit mass resolution mass spectrometers.
