自动索氏提取-高效液相色谱法同时测定油炸面制品中的16种多环芳烃

采用自动索氏提取法以丙酮:正己烷(1 : 1)混合溶液提取油炸面制品中的乡环芳烃(PAHs),以硅胶固相萃取柱净化,二氯甲烷:正己烷(5:6)洗脱,建立了同时测定油炸面制品中16种PAHs的高效液相色谱-紫外和荧光检测器测定方法.实验结果,在50μg/kg添加水平,PAHs各化合物的回收率为92.5%～106.4%,相对标准偏差(RSD)小于3.21%.16种PAHs化合物检出限为0.8μg/kg～40μg/kg.该方法简便、快速、可同时检测油炸面制品中16种PAHs.     

超高效液相色谱-串联质谱测定食品中碱性桃红T染料

建立了用超高效液相色谱-串联质谱检测食品中非法添加物碱性桃红T染料的方法.样品经80%碱化甲醇提取,在碱性条件下用聚酰胺固相萃取小柱富集、净化,并经酸化甲醇洗脱后通过超高效液相色谱-串联四极杆质谱仪检测.液相色谱条件:分离柱为Waters Acquity BEHC18柱(1.7μm,2.1 mm×100 mm);流动相为0.4%甲酸水溶液-纯甲醇;流速0.3 mL.min-1.碱性桃红T的检测限为0.3μg.kg-1,6种食品样品的回收率为83.9%~92.5%,相对标准偏差(RSD)为5.6%~8.3%(n=6).在16~800μg.kg-1浓度范围内呈良好的线性关系,线性回归系数r为0.996 6.     

超高效液相色谱-质谱联用法测定水产品中喹乙醇代谢物残留量

建立了水产品中喹乙醇代谢物残留量的超高效液相色谱-质谱联用测定方法。样品经乙酸乙酯提取、液液萃取净化后吹干,流动相定容,经超高效液相色谱分离后进入串联质谱检测器。采用电喷雾正离子,多反应监测(MRM)模式检测,内标法定量。方法的检出限为1μg/kg,浓度在2～100 ppb范围内,线性良好(r=0.999),添加浓度1～20μg/kg下,不同水产品基质的回收率在80%～100%之间,相对标准偏差(RSD)小于10%。     

凝胶渗透色谱-固相萃取-高效液相色谱法测定油脂及油炸食品中的酚类抗氧化剂

建立了使用凝胶渗透色谱-固相萃取-高效液相色谱(GPC-SPE-HPLC)测定油脂及油炸食品中的4种常见酚类抗氧化剂没食子酸丙酯(PG)、叔丁基对苯二酚(TBHQ)、叔丁基对羟基茴香醚(BHA)和二丁基羟基甲苯(BHT)的方法.试样经乙酸乙酯-环己烷(V(乙酸乙酯)∶V(环已烷)=1∶1)和乙腈漩涡振荡萃取,凝胶渗透色谱(GPC)和HLB固相萃取柱净化,以乙腈-体积分数为0.1%甲酸水溶液为流动相,以BDS HYPERSIL C18柱作为分离柱,在检测波长280nm下用紫外检测器检测.方法的检出限为0.6～1.0mg/kg(油脂样品)和0.3～0.5mg/kg(油炸样品),定量限为2～3mg/kg(油脂样品)和1～1.7mg/kg(油炸样品),线性相关系数r>0.998,平均回收率为80.3%～94.0%(油脂样品)和80.3%～93.4%(油炸样品);相对标准偏差(RSD)为3.22%～8.80%(油脂样品)和2.74%～9.62%(油炸样品).该方法选择性好,灵敏度高,检出限低,能够成功地应用于油脂及油炸食品中4种常见酚类抗氧化剂的检测.     

固相萃取—高效液相色谱法测定植物油中苯并(a)芘

本实验建立了基于固相萃取的高效液相色谱法测定植物油中苯并(a)芘含量。样品用正己烷溶解,经Cleanert BAP-3固相萃取小柱净化,采用C18色谱柱分离,以乙腈/水=80/20(V/V)为流动相,经荧光检测器检测。结果表明苯并(a)芘在0.50μg/L~50μg/L浓度范围内线性良好,相关系数为0.9999,方法检出限为0.1μg/kg,样品加标回收率为89.00%~94.46%,RSD为1.0%~2.2%。该方法具有快速、准确、灵敏、简单等特点,可用于植物油中苯并芘的检测。     

超高效液相色谱-串联质谱法检测禽畜肉中的氯霉素残留

 研究了一种针对禽畜肉中氯霉素残留量的超高效液相色谱-串联质谱联用分析方法.本方法采用乙酸乙酯萃取禽畜肉中的氯霉素,提取液氮吹至干后用超纯水溶解样品残渣,然后用HLB小柱进行固相萃取,经过净化的样品通过超高效液相色谱进行分离,然后用电喷雾质谱负离子多反应监测模式对氯霉素进行检测.该方法的检出限为0.0025μg/kg,添加水平为0.1~5.0μg/kg时,加标回收率为75.8%~82.5%,相对标准偏差小于10%.该方法具有灵敏度高、选择性好、分析时间短等优点.     

SPE-HPLC法测定环境水样中3种痕量抗生素的含量

建立了一种固相萃取-高效液相色谱法同时测定水体中氧氟沙星、四环素、磺胺甲噁唑浓度。样品经固相萃取小柱富集净化、超纯水-乙腈(75∶25,体积比)洗脱后,用高效液相色谱-紫外检测器测定。检测波长λ为274 nm,柱温30℃,流动相为乙腈-磷酸水溶液(50∶50,体积比),采用梯度洗脱程序,实现了3种待测组分的基线分离,线性范围为氧氟沙星0.25~2μg/mL,四环素0.4~2μg/mL,磺胺甲噁唑0.04~2μg/mL。空白加标回收率范围分别为82.32%~94.86%。氧氟沙星、四环素、磺胺甲噁唑的检出限分别为0.04、0.25、0.01μg/mL,定量限分别为0.25、0.40、0.04μg/mL。该方法具有快速简便、灵敏高效等优点,可满足实际工作的需要。     

磁性石墨烯-液质联用测定鸡肉中万古霉素和喹诺酮

建立了鸡肉中万古霉素和喹诺酮类药物残留的磁性石墨烯固相萃取-液相色谱-串联质谱分析方法.样品采用乙腈提取,磁性石墨烯粉分散固相萃取净化,经Agilent ZORBAX SB-C18(3.0 mm ×100.0 mm,1.8 μm)色谱柱分离,液相色谱-串联质谱仪进行检测.目标物在2.0~50.0 μg/L内线性关系良好(r²>0.99).鸡肉基质中目标化合物在5、10、25 μg/kg加标水平的回收率为71.2%~98.8%,相对标准偏差(RSD)为6.8%~14.3%.该方法净化效果好,回收率高,精密度好,可用于鸡肉中万古霉素和喹诺酮类药物残留检测.     

SPE-UPLC-MS/MS快速测定豆制品中的乌洛托品

建立了一种固相萃取-超高效液相色谱质谱联用(SPE-UPLC-MS/MS)测定豆制品中乌洛托品的分析方法。样品经粉碎后,采用乙腈提取,ProElut PXA小柱净化,Shim-pack XR-ODS色谱柱分离,在电喷雾正离子模式下用质谱仪进行MRM分析。结果表明:乌洛托品在0～160μg/kg范围内呈现良好的线性关系,线性相关系数为0.9998,该方法对应的检出限和定量限分别为0.3μg/kg和1μg/kg在5～100μg/kg添加水平下,乌洛托品回收率为88.4%～97.1%,相对标准偏差为5.39%～8.74%。该方法简便,快速,可成功应用于豆制品中乌洛托品的检测。     

地下水中多菌灵残留的SPE-HPLC分析方法

建立了检测地下水中多菌灵残留量的固相萃取-高效液相色谱法.样品经C18固相萃取小柱富集净化后,以甲醇-(水+氨水)为流动相,高效液相色谱-紫外检测器检测,外标法定量.在0.01~1.0 mg/L质量浓度范围内,线性相关系数0.999 9,最低检出限为0.003 4 mg/L.添加质量浓度为0.01,0.05,0.18 mg/L,回收率在95.3%~97.8%之间,相对标准偏差(RSD)为3.09%~4.18%.方法应用在实际样品分析中可行,适用于地下水样中痕量有机物的检测.     

Characterization of Ordovician carbonate reservoirs, southeastern Saskatchewan, Canada

The discovery of the prolific Ordovician Red River reservoirs in 1995 in southeastern Saskatchewan was the catalyst for extensive exploration activity which resulted in the discovery of more than 15 new Red River pools. The best yields of Red River production to date have been from dolomite reservoirs. Understanding the processes of dolomitization is, therefore, crucial for the prediction of the connectivity, spatial distribution and heterogeneity of dolomite reservoirs.The Red River reservoirs in the Midale area consist of 3～4 thin dolomitized zones, with a total thickness of about 20 m, which occur at the top of the Yeoman Formation. Two types of replacement dolomite were recognized in the Red River reservoir: dolomitized burrow infills and dolomitized host matrix. The spatial distribution of dolomite suggests that burrowing organisms played an important role in facilitating the fluid flow in the backfilled sediments. This resulted in penecontemporaneous dolomitization of burrow infills by normal seawater. The dolomite in the host matrix is interpreted as having occurred at shallow burial by evaporitic seawater during precipitation of Lake Almar anhydrite that immediately overlies the Yeoman Formation. However, the low δ18O values of dolomited burrow infills (-5.9‰～ -7.8‰, PDB) and matrix dolomites (-6.6‰～ -8.1‰, avg. -7.4‰ PDB) compared to the estimated values for the late Ordovician marine dolomite could be attributed to modification and alteration of dolomite at higher temperatures during deeper burial, which could also be responsible for its 87Sr/86Sr ratios (0.7084～0.7088) that are higher than suggested for the late Ordovician seawaters (0.7078～0.7080). The trace amounts of saddle dolomite cement in the Red River carbonates are probably related to "cannibalization" of earlier replacement dolomite during the chemical compaction.     

A computer generator for randomly layered structures

AcomputergeneratorforrandomlylayeredstructuresYUJia shun1,2,HEZhen hua2(1.TheInstituteofGeologicalandNuclearSciences,NewZealand;2.StateKeyLaboratoryofOilandGasReservoirGeologyandExploitation,ChengduUniversityofTechnology,China)Abstract:Analgorithmisintrod…     

海南岛地体及其毗邻陆缘晚中生代—新生代古地磁研究和构造演化

本文叙述了对海南岛及其毗邻大陆边缘白垩纪到第四纪地层岩石进行古地磁研究的全部工作过程。通过分析岩石中剩余磁矢量的磁偏角及磁倾角的变化,提出海南岛白垩纪以来经历的构造演化模式如下:早期伴随顺时针旋转而向南迁移,后期伴随逆时针转动并向北运移。联系该地区及邻区的地质、地球物理资料,对海南岛上述的构造地体运动提出以下认识:北部湾内早期有一拉张作用,主要是该作用使湾内地壳显著伸长减薄,形成北部湾盆地。从而导致了海南岛的早期构造运动,而海南岛后期的构造运动则主要是受南海海底扩张的影响。海南地体运动规律的阐明对于了解北部湾油气盆地的形成演化有重要的理论和实际意义。     

Exciton Seebeck in Molecular Systems

Various applications relevant to the exciton dynamics,such as the organic solar cell,the large-area organic light-emitting diodes and the thermoelectricity,are operating under temperature gradient.The potential abnormal behavior of the exicton dynamics driven by the temperature difference may affect the efficiency and performance of the corresponding devices.In the above situations,the exciton dynamics under temperature difference is mixed with     

Achieving Unusual States of Matter Under High Pressure

The elongation method,originally proposed by Imamura was further developed for many years in our group.As a method towards O(N)with high efficiency and high accuracy for any dimensional systems.This treatment designed for one-dimensional(ID)polymers is now available for three-dimensional(3D)systems,but geometry optimization is now possible only for 1D-systems.As an approach toward post-Hartree-Fock,it was also extended to     

《Chinese Science Bulletin》SUBJECT INDEX TO VOLUME 59(2014)

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An on-line scaling method for improving scalability of a database cluster

The explosive growth of the Internet and database applications has driven database to be more scalable and available, and able to support on-line scaling without interrupting service. To support more client's queries without downtime and degrading the response time, more nodes have to be scaled up while the database is running. This paper presents the overview of scalable and available database that satisfies the above characteristics. And we propose a novel on-line scaling method. Our method improves the existing on-line scaling method for fast response time and higher throughputs. Our proposed method reduces unnecessary network use, i.e. , we decrease the number of data copy by reusing the backup data. Also, our on-line scaling operation can be processed parallel by selecting adequate nodes as new node. Our performance study shows that our method results in significant reduction in data copy time.     

An improved R-tree based on childnode''s probability

R-Tree is a good structure for spatial searching. But in this indexing structure,either the sequence of nodes in the same level or sequence of traveling these nodes when queries are made is random. Since the possibility that the object appears in different MBR which have the same parents node is different, if we make the subnode who has the most possibility be traveled first, the time cost will be decreased in most of the cases. In some case, the possibility of a point belong to a rectangle will shows direct proportion with the size of the rectangle. But this conclusion is based on an assumption that the objects are symmetrically distributing in the area and this assumption is not always coming into existence. Now we found a more direct parameter to scale the possibility and made a little change on the structure of R-tree, to increase the possibility of founding the satisfying answer in the front sub trees. We names this structure probability based arranged R-tree (PBAR-tree).     

An Index mechanism for multi-scale view in spatial databases

There are numerous geometric objects stored in the spatial databases. An importance function in a spatial database is that users can browse the geometric objects as a map efficiently. Thus the spatial database should display the geometric objects users concern about swiftly onto the display window. This process includes two operations:retrieve data from database and then draw them onto screen. Accordingly, to improve the efficiency, we should try to reduce time of both retrieving object and displaying them. The former can be achieved with the aid of spatial index such as R-tree, the latter require to simplify the objects. Simplification means that objects are shown with sufficient but not with unnecessary detail which depend on the scale of browse. So the major problem is how to retrieve data at different detail level efficiently. This paper introduces the implementation of a multi-scale index in the spatial database SISP (Spatial Information Shared Platform) which is generalized from R-tree. The difference between the generalization and the R-tree lies on two facets: One is that every node and geometric object in the generalization is assigned with a importance value which denote the importance of them, and every vertex in the objects are assigned with a importance value,too. The importance value can be use to decide which data should be retrieve from disk in a query. The other difference is that geometric objects in the generalization are divided into one or more sub-blocks, and vertexes are total ordered by their importance value. With the help of the generalized R-tree, one can easily retrieve data at different detail levels.Some experiments are performed on real-life data to evaluate the performance of solutions that separately use normal spatial index and multi-scale spatial index. The results show that the solution using multi-scale index in SISP is satisfying.     

Integrating GIS Web services based on mediating architecture

The geographic information service is enabled by the advancements in general Web service technology and the focused efforts of the OGC in defining XML-based Web GIS service. Based on these models, this paper addresses the issue of services chaining,the process of combining or pipelining results from several interoperable GIS Web Services to create a customized solution. This paper presents a mediated chaining architecture in which a specific service takes responsibility for performing the process that describes a service chain. We designed the Spatial Information Process Language (SIPL) for dynamic modeling and describing the service chain, also a prototype of the Spatial Information Process Execution Engine (SIPEE) is implemented for executing processes written in SIPL. Discussion of measures to improve the functionality and performance of such system will be included.