[目的]建立QuEChERS结合UPLC-MS/MS法测定海南豇豆中倍硫磷及其Ⅰ型代谢物的分析方法。[方法]样品经乙腈提取,氯化钠盐析,石墨化炭黑(GCB)和N-丙基乙二胺(PSA)分散固相萃取净化,以Agilent ZORBAX Eclipse Plus C18柱为分离色谱柱,多反...[目的]建立QuEChERS结合UPLC-MS/MS法测定海南豇豆中倍硫磷及其Ⅰ型代谢物的分析方法。[方法]样品经乙腈提取,氯化钠盐析,石墨化炭黑(GCB)和N-丙基乙二胺(PSA)分散固相萃取净化,以Agilent ZORBAX Eclipse Plus C18柱为分离色谱柱,多反应监测(MRM)模式下检测倍硫磷及其Ⅰ型代谢物,定量分析采用溶剂标准曲线法(外标法)。[结果]倍硫磷及其Ⅰ型代谢物在2.0~100.0μg/L质量浓度范围内线性关系良好,相关系数(r)大于0.999;以海南豇豆阴性样品为基质,在2、5、10、50μg/kg 4个质量分数加标水平下,倍硫磷及其Ⅰ型代谢物的平均加标回收率为89.3%~99.3%,相对标准偏差(RSD)为1.2%~7.3%,方法定量限均为2μg/kg。[结论]方法具有简便、高效、准确、廉价等特点,适用于豇豆中倍硫磷及其Ⅰ型代谢物的同时测定。方法的建立可为相关监管部门对豇豆中倍硫磷及其Ⅰ型代谢物农药污染的有效监测提供技术支撑。展开更多
Introduction Aconitine-type alkaloids isolated from the roots of Aconitum carmiechaeli show a potential toxicity and a broad spectrum of bioactivity[1-4].On the basis of the C8-substituent of C19-diterpenoid skeleton,...Introduction Aconitine-type alkaloids isolated from the roots of Aconitum carmiechaeli show a potential toxicity and a broad spectrum of bioactivity[1-4].On the basis of the C8-substituent of C19-diterpenoid skeleton,aconitine-type alkaloids can be divided into diester-diterpenoid alkaloids（DDAs）,monoester-diterpenoid alkaloids（MDAs）,and lipo-alkaloids（Fig.1）.展开更多
The Kunlunguan biotite granite pluton, located in the southwestern part of the Nanling Mesozoic granite belt, is controlled by the NW-trending Nandan-Kunlunguan deep fault. LA-ICP-MS zircon U-Pb dating yielded a weigh...The Kunlunguan biotite granite pluton, located in the southwestern part of the Nanling Mesozoic granite belt, is controlled by the NW-trending Nandan-Kunlunguan deep fault. LA-ICP-MS zircon U-Pb dating yielded a weighted mean 206Pb/238U age of 93.0±1 Ma (MSDW=1.7) for the main part of the pluton, implying its Late Creta-ceous intrusion. The Kunlunguan body is a high-K calc-alkaline rock characterized by high silicon, alkali and alu-minum, and low phosphorus and titanium. SiO2 contents of the Kunlunguan body range from 68.13% to 72.61% and K2O/Na2O ratios from 1.28 to 1.87. A/CNK values vary from 0.76 to 1.42, indicating a metaluminous to intensively peraluminous character. The rocks are enriched in Ga, Rb, Th, U and Pb but depleted in Ba, Nb, Sr, P and Ti. The REEs are characterized by remarkable negative Eu anomalies (Eu/Eu*=0.53-0.73) and exhibit right-inclined "V"-shaped patterns with LREE enrichment. Petrology, major and trace elements data all indicate that the pluton is aluminous A-type granite which intruded in a post-collisional extensional tectonic setting. It is related to back-arc extension, reflecting high-angle subduction of the paleo-Pacific plate, caused by northward movement of the Indian plate. The Nandan-Kunlunguan A-type granites belt, together with similar plutons in the coastal areas of Zhejiang and Fujian provinces, represent the two A-type granite belts under a matching tectonic system.展开更多
链霉菌种类繁多,以盛产抗生素而闻名,是极具研发价值的放线菌类群。然而,商业数据库中收录的链霉菌属菌种数量较少,这限制了基质辅助激光解吸电离飞行时间质谱(matrix-assisted laser desorption/ionization-time of flight mass spectr...链霉菌种类繁多,以盛产抗生素而闻名,是极具研发价值的放线菌类群。然而,商业数据库中收录的链霉菌属菌种数量较少,这限制了基质辅助激光解吸电离飞行时间质谱(matrix-assisted laser desorption/ionization-time of flight mass spectrometry,MALDI-TOF MS)技术在链霉菌鉴定中的应用。【目的】基于全基因组测序数据挖掘,建立链霉菌属菌种的MALDI-TOF MS数据库,并测试其准确性。【方法】检索基因组数据库,提取已测序的链霉菌属菌种模式菌株的12种核糖体蛋白序列,并计算其理论MALDI质谱峰值,以这12个峰值的组合作为菌种鉴定依据建立数据库。收集模式菌株进行MALDI-TOF MS测试,将实测峰值与数据库中菌种的理论峰值进行比对,以测试建库方法及数据库比对结果的准确性。【结果】建立了包含链霉菌属615个菌种的MALDI-TOF MS数据库。测试菌株的质谱均实现了与数据库中目标菌种的准确匹配。本研究还提出了基于数据库比对的菌种鉴定方法。【结论】本研究建立的数据库为基于MALDI-TOF MS技术鉴定链霉菌奠定了基础。展开更多
目的旨在建立一种基于生物传感器联合超高效液相色谱/串联质谱(ultra-performance liquid chromatography with electrospray tandem mass spectrometry,UPLC-MS/MS)的中药苦味关键质量属性辨识方法。以白术内酯类成分为研究对象,通过...目的旨在建立一种基于生物传感器联合超高效液相色谱/串联质谱(ultra-performance liquid chromatography with electrospray tandem mass spectrometry,UPLC-MS/MS)的中药苦味关键质量属性辨识方法。以白术内酯类成分为研究对象,通过分子对接与生物传感技术揭示其与苦味受体的相互作用机制,实现苦味属性从传统经验判定到分子水平表征的跨越,为完善白术质量控制体系提供支撑。方法采用D101大孔吸附树脂结合紫外分光光度法,制备并筛选富含内酯类成分的白术组分;通过UPLC-MS/MS与分子对接技术,在分子水平解析白术组分与味觉受体的相互作用特征;采用生物传感器与UPLCMS/MS联用技术,实现白术组分苦味关键质量属性的精准辨识。结果成功制得白术不同极性组分11个,其中白术醇提物70%组分的总内酯含量最高,为后续性味研究的理想载体;分子对接实验显示白术组分与Ⅱ型味觉受体家族14号成员(taste receptor type 2 member 14,TAS2R14)的结合展现出明显优势,在分子层面揭示了白术组分具有强烈趋于苦味属性的作用特质;进一步构建苦味生物传感器,对白术组分的苦味属性进行表征,结果显示白术组分与TAS2R14的相互结合强度为49.0ng/L,属于强相互作用,表明以内酯类成分为主的白术组分具有显著的苦味属性,该结果与分子对接结果相互印证,增强了实验结论的可靠性;最后,联合UPLC-MS/MS技术,共辨识得到包括白术内酯Ⅱ在内的苦味关键质量属性13个,在物质基础层面表明白术组分与苦味受体TAS2R14的结合受关键质量属性驱动,为理解白术内酯类成分苦味特性提供直接证据。结论通过多技术融合的系统性研究,从分子相互作用到物质基础层面揭示了白术内酯类成分苦味属性的本质,所发现的苦味关键质量属性为建立基于苦味特征的白术质量控制方法奠定了理论基础,此外,提出的技术路线为中药苦味物质基础研究提供了新的方法学参考。展开更多
基金Supported by the National Natural Science Foundation of China(Nos.30472134and30672600)the National Basic Re-search Program of China(No.2006CB5047060).
文摘Introduction Aconitine-type alkaloids isolated from the roots of Aconitum carmiechaeli show a potential toxicity and a broad spectrum of bioactivity[1-4].On the basis of the C8-substituent of C19-diterpenoid skeleton,aconitine-type alkaloids can be divided into diester-diterpenoid alkaloids（DDAs）,monoester-diterpenoid alkaloids（MDAs）,and lipo-alkaloids（Fig.1）.
基金supported by the Program for Changjiang Schoolars and Innovative Research Team in University (IRT0755)the Key Laboratory of Geological Progress and Mineral Resources (GPMR),China University of Geosciences
文摘The Kunlunguan biotite granite pluton, located in the southwestern part of the Nanling Mesozoic granite belt, is controlled by the NW-trending Nandan-Kunlunguan deep fault. LA-ICP-MS zircon U-Pb dating yielded a weighted mean 206Pb/238U age of 93.0±1 Ma (MSDW=1.7) for the main part of the pluton, implying its Late Creta-ceous intrusion. The Kunlunguan body is a high-K calc-alkaline rock characterized by high silicon, alkali and alu-minum, and low phosphorus and titanium. SiO2 contents of the Kunlunguan body range from 68.13% to 72.61% and K2O/Na2O ratios from 1.28 to 1.87. A/CNK values vary from 0.76 to 1.42, indicating a metaluminous to intensively peraluminous character. The rocks are enriched in Ga, Rb, Th, U and Pb but depleted in Ba, Nb, Sr, P and Ti. The REEs are characterized by remarkable negative Eu anomalies (Eu/Eu*=0.53-0.73) and exhibit right-inclined "V"-shaped patterns with LREE enrichment. Petrology, major and trace elements data all indicate that the pluton is aluminous A-type granite which intruded in a post-collisional extensional tectonic setting. It is related to back-arc extension, reflecting high-angle subduction of the paleo-Pacific plate, caused by northward movement of the Indian plate. The Nandan-Kunlunguan A-type granites belt, together with similar plutons in the coastal areas of Zhejiang and Fujian provinces, represent the two A-type granite belts under a matching tectonic system.
文摘目的旨在建立一种基于生物传感器联合超高效液相色谱/串联质谱(ultra-performance liquid chromatography with electrospray tandem mass spectrometry,UPLC-MS/MS)的中药苦味关键质量属性辨识方法。以白术内酯类成分为研究对象,通过分子对接与生物传感技术揭示其与苦味受体的相互作用机制,实现苦味属性从传统经验判定到分子水平表征的跨越,为完善白术质量控制体系提供支撑。方法采用D101大孔吸附树脂结合紫外分光光度法,制备并筛选富含内酯类成分的白术组分;通过UPLC-MS/MS与分子对接技术,在分子水平解析白术组分与味觉受体的相互作用特征;采用生物传感器与UPLCMS/MS联用技术,实现白术组分苦味关键质量属性的精准辨识。结果成功制得白术不同极性组分11个,其中白术醇提物70%组分的总内酯含量最高,为后续性味研究的理想载体;分子对接实验显示白术组分与Ⅱ型味觉受体家族14号成员(taste receptor type 2 member 14,TAS2R14)的结合展现出明显优势,在分子层面揭示了白术组分具有强烈趋于苦味属性的作用特质;进一步构建苦味生物传感器,对白术组分的苦味属性进行表征,结果显示白术组分与TAS2R14的相互结合强度为49.0ng/L,属于强相互作用,表明以内酯类成分为主的白术组分具有显著的苦味属性,该结果与分子对接结果相互印证,增强了实验结论的可靠性;最后,联合UPLC-MS/MS技术,共辨识得到包括白术内酯Ⅱ在内的苦味关键质量属性13个,在物质基础层面表明白术组分与苦味受体TAS2R14的结合受关键质量属性驱动,为理解白术内酯类成分苦味特性提供直接证据。结论通过多技术融合的系统性研究,从分子相互作用到物质基础层面揭示了白术内酯类成分苦味属性的本质,所发现的苦味关键质量属性为建立基于苦味特征的白术质量控制方法奠定了理论基础,此外,提出的技术路线为中药苦味物质基础研究提供了新的方法学参考。
