液相色谱—串联质谱法检测蜂王浆中三环锡残留量

本实验研究建立了蜂王浆中三唑锡残留量的液相色谱-质谱串联检测方法.三环环锡经过酸化乙腈提取,经固相萃取柱,C-18色谱柱梯度洗脱分离,取365.1→201.1,365.1→283.2,365.1→219.1 m/z为主要特征离子365.1→201.1 m/z为定量离子,以三重四级杆为质量检测器检测三环锡的方法.该方法线性范围:1-50 ng/g,仪器检出限:1 ng/g;添加浓度20 ng/g、25 ng/g、50 ng/g回收率:80％～105％,相对标准偏差3.9％～8.8％.     

液相色谱-串联质谱法同时快速测定婴幼儿谷物食品中3种莨菪烷生物碱

采用固相萃取净化去除样品中蛋白类物质的干扰,建立婴幼儿谷物食品中3种莨菪烷生物碱的液相色谱-串联质谱检测方法.样品经体积分数为80％(v/v)乙腈水溶液提取后,经Oasis PRiME HLB SPE固相萃取柱净化.净化后的样品采用Agilent Poroshell 120 EC-C18柱(2.7μm,3.0 mm×75 mm)分离,以0.1％(v/v)甲酸乙腈溶液和0.1％(v/v)甲酸水溶液为流动相,梯度洗脱,多反应监测正离子模式扫描,采用基质溶液外标法定量.3种莨菪烷生物碱在1.0～50.0μg·L-1浓度范围内线性关系良好(R2﹥0.999),方法的检出限均为0.5μg·kg-1;回收率为86.8％ ～103.3％,相对标准偏差为5.2％ ～8.9％.该方法前处理操作简便,灵敏度和准确度高,可实现婴幼儿谷物食品中3种莨菪烷生物碱的同时快速测定.     

HPLC/MS/MS法同时测定小鼠血浆中人参皂苷Rg1、Re、Rb1

利用高效液相色谱-串联质谱联用的技术,建立同时测定小鼠血浆中的人参皂苷Rg1、Re、Rb1浓度的分析方法.以RESTEK PinnacleⅡC18柱(50 mm×2.1 mm,5 μm)为色谱柱,流动相:乙腈-水(梯度洗脱);流速200 μL·min-1;柱温:20 ℃;质谱条件为气动辅助电喷雾离子源(ESI),检测方式为正离子多离子反应监测(MRM),用于定量分析的离子为m/z Rg1 832.8→643.6;Re 969.8→789.7;Rb11132.1→365.3;生物样品采用固相萃取方法处理.人参皂苷Rg1、Re、Rb1标准曲线的线性范围为0.5～1 000 ng·mL-1,最低定量下限达到0.5 ng·mL-1,日内、日间变异系数(RSD)均<15%,精密度和准确度等均符合生物样品分析的要求.结果表明该法准确、灵敏、特异,适用于血浆中人参皂苷Rg1、Re、Rb1浓度的同时测定.     

高效液相色谱-串联质谱法对贯叶连翘中4种黄酮醇类化合物抗氧化活性的定量研究*

建立了高效液相色谱-串联质谱(HPLC-ESI/MS)法对芦丁、金丝桃苷、槲皮素和槲皮苷的抗氧化活性进行定量研究。样品用甲醇溶解,采用Hewlett Packard ODS Hypersil C_(18)色谱柱(100 mm×4.6 mm,5μm)、0.1%甲酸水-甲醇为流动相梯度洗脱,流速0.6 m L·min~(-1),柱温25℃;电喷雾源,负离子模式多反应选择离子检测(MRM),用于定性、定量的母离子和子离子分别为m/z 609→300(芦丁)、m/z 463→300(金丝桃苷)、m/z 301→151(槲皮素)、m/z 447→300(槲皮苷),采用外标法进行定量分析。结果表明:芦丁、金丝桃苷、槲皮素和槲皮苷在0.5~1 600 ng·mL~(-1)范围内线性关系良好(R0.998),定量限为0.5 ng·m L~(-1),仪器精密度良好(RSD3.0%),样品反应液在24 h内稳定性良好。本方法具有灵敏度高,分析时间短等特点,相对于其他检测方法,提高了检测的准确性,适用于对贯叶连翘中黄酮醇类化合物抗氧化活性的定量研究。经计算,芦丁、金丝桃苷、槲皮素和槲皮苷对ABTS~(.+)的清除率分别为18.35%、36.28%、41.50%和37.18%。     

液相色谱—串联质谱法测定中华绒螯蟹中21种磺胺类药物残留

建立了一种液相色谱-电喷雾串联质谱同时测定中华绒螯蟹中21种磺胺类药物残留的方法.均质样品先后用乙腈、二氯甲烷提取,合并提取液,取部分提取液经氮吹浓缩.残渣用1 mL流动相溶解,饱和正己烷脱脂净化.采用ZOR-BAX Eclipse XDB-C8色谱柱,以含0.2%乙酸的水溶液和甲醇(7:3)为流动相,梯度洗脱,在电喷雾-多反应监测离子模式下,进行定量定性分析.方法的定量限为5μg/kg;以标准加入法计算回收率,在4～40μg/kg添加范围内,平均回收率为71.8%～106%;相对标准偏差为0.44%～10.1%.     

高效液相色谱法测定人血浆中硫普罗宁的浓度

建立了以反相高效液相色谱法测定人血浆中硫普罗宁浓度的方法.采用Agilent C8 (250 mm×4.6 mm,5μm)色谱柱,乙腈:水(用磷酸调pH至2.5) =8:92(v/v),为流动相,检测波长203 nm,流速1.0 mL·min-1.硫普罗宁浓度在1.5～1 600 μg·mL-1浓度范围内,峰面积与浓度...     

亲水作用毛细管电色谱分析苷类药物的研究

基于多面体寡聚硅倍半氧烷-甲基丙烯酸羟乙酯poly(POSS-MA-co-HEMA)有机硅胶杂化整体柱,建立典型苷类药物(连翘苷、豆腐果苷、紫丁香苷、天麻素)的亲水作用毛细管电色谱检测技术.考察流动相乙腈比例、缓冲液浓度、缓冲溶液p H值、分离电压和反压阀压力对四种苷类药物分离效果的影响,在最优条件下(流动相为2 mmol·L-1磷酸三乙胺缓冲液(乙腈体积分数为90%,p H=7.0),分离电压-8 k V、柱压力5.4MPa),4种苷类药物在10 min内得到了基线分离.连翘苷、豆腐果苷、紫丁香苷和天麻素线性范围分别为10~200、25~200、15~200和25~200μg·m L-1,检测限为1.5~8.0μg·m L-1.应用于血清模拟样品分析,平均回收率为95.6%~99.1%,相对标准偏差小于3.3%.     

反相离子对色谱法测定手性生物转化中扁桃酸与苯乙酮酸

建立一种同时测定生物不对称转化发酵液中扁桃酸及苯乙酮酸含量的反相离子对高效液相色谱方法.色谱柱为HypersilC18柱(4.6mm×250mm,5μm),流动相为甲醇-25mmol·L-1磷酸二氢钾缓冲液(内含6mmol·L-1四丁基溴化铵,NaOH调pH至7.0)(体积分数15∶85),流速为1.0mL·min-1,检测波长220nm,柱温为室温.扁桃酸与苯乙酮酸在0.5～20mmol·L-1内,其浓度与峰面积呈现良好的线性关系(r=0.9994,0.9997).二者的加样回收率均为96.5%～100.6%.当信噪比(S/N)为3时,二者的最低检测浓度分别为2.4和8μmol·L-1.该方法简便、准确、灵敏度高,可用于手性生物转化中扁桃酸与苯乙酮酸的定量分析.     

匀浆法提取-离子色谱法测定卷烟纸中钾、钠、钙、镁

研究了用离子色谱法同时测定卷烟纸中钾、钠、钙、镁.卷烟纸用1%的盐酸溶液匀浆法提取,然后以Ionpac CS16(5mm×250mm,5μm)离子交换柱为固定相,0.03mol/L甲烷磺酸为流动相分离,电导检测器检测测定,方法的检出限为1.8～6.5μg·L-1,加标回收率为94%～104%,相对标准偏差为0.84%～1.2%,结果满意.     

用超高效液相色谱串联质谱法测定全血中的野麦枯

建立超高效液相色谱串联质谱法(UPLC-MS/MS)测定全血中的野麦枯的方法。样品血经pH=8氨水稀释后,涡旋离心,上清液过混合型弱阳离子交换柱(WCX)纯化,采用UPLC-MS/MS检测。质谱检测采用正离子扫描,多反应离子监测模式(MRM)。以野麦枯母离子248.85(m/z)和子离子130.13及192.95(m/z)定性和定量。加标回收率为77.61%~81.22%,检出限为1 ng/mL。该方法灵敏度高,分析速度快,操作简便。     

Markedness and its Interpretation in Language Use

Language markedness is a common phenomenon in languages, and is reflected from hearing, vision and sense, i.e. the variation in the three aspects such as phonology, morphology and semantics. This paper focuses on the interpretation of markedness in language use following the three perspectives, i.e. pragmatic interpretation, psychological interpretation and cognitive interpretation, with an aim to define the function of markedness.     

Lower Paleozoic oil relationships within Williston Basin, Canada

The Williston Basin is a significant petroleum province, containing oil production zones that include the Middle Cambrian to Lower Ordovician, Upper Ordovician, Middle Devonian, Upper Devonian and Mississippian and within the Jurassic and Cretaceous. The oils of the Williston Basin exhibit a wide range of geochemical characteristics defined as "oil families", although the geochemical signature of the Cambrian Deadwood Formation and Lower Ordovician Winnipeg reservoired oils does not match any "oil family". Despite their close stratigraphic proximity, it is evident that the oils of the Lower Palaeozoic within the Williston Basin are distinct. This suggests the presence of a new "oil family" within the Williston Basin. Diagnostic geochemical signatures occur in the gasoline range chromatograms, within saturate fraction gas chromatograms and biomarker fingerprints. However, some of the established criteria and cross-plots that are currently used to segregate oils into distinct genetic families within the basin do not always meet with success, particularly when applied to the Lower Palaeozoic oils of the Deadwood and Winnipeg Formation.     

An Analysis of Catherine＇s Character——Wuthering Heights

Wuthering Heights, Emily Bronte＇s only novel, was published in December of 1847 under the pseudonym Ellis Bell. The book did not gain immediate success, but it is now thought one of the finest novels in the English language. Catherine is the key character of this masterpiece, because everybody and everything center on her though she had a short life. We can understand this masterpiece better if we know Catherine well.     

Features of Women's language

Language is a means of verbal communication. People use language to communicate with each other. In the society, no two speakers are exactly alike in the way of speaking. Some differences are due to age, gender, statue and personality. Above all, gender is one of the obvious reasons. The writer of this paper tries to describe the features of women＇s language from these perspectives： pronunciation, intonation, diction, subjects, grammar and discourse. From the discussion of the features of women＇s language, more attention should be paid to language use in social context. What＇s more, the linguistic phenomena in a speaking community can be understood more thoroughly.     

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.     

Design and analysis of generic LBS application developing platform

Location based services is promising due to its novel working style and contents.A software platform is proposed to provide application programs of typical location based services and support new applications developing efficiently. The analysis shows that this scheme is easy implemented, low cost and adapt to all kinds of mobile nework system.     

橡胶颗粒沥青混合料低温抗裂性试验研究

以AC-13级配为基础,将橡胶颗粒代替部分集料掺入混合料中,以低温弯曲试验为评价方法对不同橡胶颗粒掺量下沥青混合料的低温抗裂性进行研究,并引入应变能密度值对混合料的低温抗裂性进行综合评价.试验结果表明:橡胶颗粒沥青混合料试件的破坏微应变均超过2 300,满足冬寒区的技术指标;无论是否掺加橡胶颗粒,随着温度的下降,沥青混合料破坏时的最大弯拉强度增大,弯拉应变降低,劲度模量增大;弯曲应变能密度在胶粒掺量为1%左右时具有较大的弯曲应变能密度值,此时橡胶颗粒沥青混合料具有较好的低温抗裂性.     

低渗透非均质砂岩油藏启动压力梯度研究

理论推导与室内实验相结合,建立了低渗透非均质砂岩油藏启动压力梯度确定方法。首先借助油藏流场与电场相似的原理,推导了非均质砂岩油藏启动压力梯度计算公式。其次基于稳定流实验方法,建立了非均质砂岩油藏启动压力梯度测试方法。结果表明:低渗透非均质砂岩油藏的启动压力梯度确定遵循两个等效原则。平面非均质油藏的启动压力梯度等于各级渗透率段的启动压力梯度关于长度的加权平均;纵向非均质油藏的启动压力梯度等于各渗透率层的启动压力梯度关于渗透率与渗流面积乘积的加权平均。研究成果可用于有效指导低渗透非均质砂岩油藏的合理井距确定,促进该类油藏的高效开发。     

On Tragic Consciousness In The Works By Ernest Hemingway

As an American modern novelist who were famous in the literary world, Hemingway was not a person who always followed the trend but a sharp observer. At the same time, he was a tragedy maestro, he paid great attention on existence, fate and end-result. The dramatis personae's tragedy of his works was an extreme limit by all means tragedy on the meaning of fearless challenge that failed. The beauty of tragedy was not produced on the destruction of life, but now this kind of value was in the impact activity. They performed for the reader about the tragedy on challenging for the limit and the death.     

Quantitative trait loci （QTLs） for quality traits related to protein and starch in wheat

Quality traits in wheat （Triticum aestirum L.） were studied by quantitative trait locus （QTL） analysis in a recombinant inbred line （RIL） population, a set of 131 lines derived from Chuan 35050 × Shannong 483 cross （ChSh）. Grains from RILs were assayed for 21 quality traits related to protein and starch. A total of 35 putative QTLs for 19 traits with a single QTL explaining 7.99-40.52% of phenotypic variations were detected on 10 chromosomes, 1D, 2A, 2D, 3B, 3D, 5A, 6A, 6B, 6D, and 7B. The additive effects of 30 QTLs were positive, contributed by Chuan 35050, the remaining 5 QTLs were negative with the additive effect contributed by Shannong 483. For protein traits, 15 QTLs were obtained and most of them were located on chromosomes 1 D, 3B and 6D, while 20 QTLs for starch traits were detected and most of them were located on chromosomes 3D, 6B and 7B. Only 7 QTLs for protein and starch traits were co-located in three regions on chromosomes 1D, 2A and 2D. These protein and starch trait QTLs showed a distinct distribution pattern in certain regions and chromosomes. Twenty-two QTLs were clustered in 6 regions of 5 chromosomes. Two QTL clusters for protein traits were located on chromosomes 1D and 3B, respectively, three clusters for starch traits on chromosomes 3D, 6B and 7B, and one cluster including protein and starch traits on chromosome 1D.