气相色谱-质谱法分析怀山药中的有机成分

以二氯甲烷为溶剂提取怀山药中的有机成分,利用气相色谱—质谱联用技术进行分析鉴定,结合计算机质谱图库检索技术对分离的化合物进行结构分析,并采用峰面积归一化法确定出各成分的相对百分含量.分析结果表明:从怀山药中共提取分离出74种化合物,鉴定出41种有机成分,占挥发性物质总含量的95.03%.主要成分为脂肪酸类、甾醇类、酯类、维生素E等,其中,含量最高的是甾醇类化合物(45%).     

城市污泥中的有机污染物的GC-MS法类型分布研究

对有机污染物的样品预处理方法和检测条件进行了探讨与优化,采用气相色谱/质谱联用法(GC-MS)对存在于沈阳三个污水处理厂产出污泥的有机污染物进行了类型分布研究.结果表明:烷烃类是满堂河污泥的主要污染物,各类有机物检出量远低于其它两种污泥;烷烃类、芳烃类和烯烃类是仙女河污泥的主要污染物,各类有机物检出量都较高.有机物污染程度比较:仙女河污泥>北部污泥>满堂河污泥,资源化利用首选满堂河污泥.三种污泥都含有美国EPA和我国优先控制有机污染物,应注意监控由于长期累积作用对土壤和地下水造成的二次污染.     

QuEChERS－GC－QqQ－MS／MS测定葡萄酒中杀菌剂残留方法研究

运用简易、高效的QuEChERS前处理方法,建立气相色谱－质谱/质谱联用法（GC－QqQ－MS/MS）检测葡萄酒中4种杀菌剂残留的分析方法．对影响前处理效果的因素进行优化,QuEChERS方法：称取10．0 g样品,加入10．0 mL乙腈,混匀1 min,4℃条件下5000 r/min离心5 min;取上清液10 mL,加入4．0 g无水硫酸镁、1．0 g氯化钠、1．37 g柠檬酸三钠、0．13 g柠檬酸,混匀1 min,4℃条件下5000 r/min离心5 min;取上清液8．0 mL,加入200 mg PSA和1200 mg无水硫酸镁,混匀1 min,4℃条件下10000 r/min离心5 min;取上清液5．0 mL,加入50μL 5％的甲酸/乙腈溶液混匀,氮气吹至近干,正己烷定容至1．0 mL,供GC－MS/MS分析．优化条件下,四种农药在0．01－6 mg/kg之间呈良好线性关系,相关系数r大于0．999,该方法的最低检出限（LOD）在0．0063－0．02 mg/kg之间．该方法简便、快速、灵敏、有机溶剂用量少,适用于葡萄酒中杀菌剂的同时分析．     

快速测定卷烟包装纸中挥发性有机化合物顶空—气相色谱/质谱联用法

卷烟包装纸中挥发性有机化合物的分析一般采用顶空—气相色谱法,该方法需分别用顶空—气相色谱/质谱联用法定性及顶空—气相色谱法定量。本方法使用顶空—气质联用法直接分析了卷烟包装纸中的15种挥发性有机化合物的含量,简化了分析步骤,且方法准确、快速、可靠。     

GC-MS法测定银杏内酯B(原料药)中石油醚残留量

作者建立了检测银杏内酯B(原料药)中石油醚(60～90℃)残留的方法.以甲醇为萃取溶剂,采用超声提取法对样品进行前处理,采用气相色谱-质谱联用法进行检测.结果表明:该法在5 min内能较好地分离石油醚的所有组分,样品的加样回收率(n=6)为98.8%,RSD为2.55%,低检测限为1.61×10-5μg.该法具有灵敏、准确、快速等特点.     

现代仪器方法在中药分析检测中的应用进展

中药具有来源、成分、配伍应用、体内转化产物多样等特点,构成了一个非常复杂的物质体系,致使其理化性质差异很大、药理活性及作用机理多样.因此在中药现代化进程中,一个重要的任务是建立合理可靠的分析检测方法,以保证中药的质量稳定可控和安全有效.文章综述了近年来中药研究与生产中常用的现代仪器分析检测方法,为中药现代化发展提供一定...     

角鲨烯软胶囊中角鲨烯的鉴定和分析

用红外光谱和质谱对角鲨烯软胶囊中的角鲨烯进行成分鉴定,用气相色谱-质谱法测定角鲨烯含量。结果表明：所建立的气相色谱-质谱定量分析方法的平均回收率为98.7%,相对标准偏差为5.9%,线性相关系数为0.9999,最低检出限为0.6ng/ml。     

黔产七叶莲挥发性成分GC-MS测定分析

为了研究黔产七叶莲药材中挥发性化学成分的组成,采用乙醇回流提取,氯仿萃取其挥发性成分,并采用GC—MS技术分析其组成。结果表明：从七叶莲氯仿萃取物中分离并鉴定出42个成分,检出率为96．338％。其中,主要含亚油酸甲酯、棕榈酸甲酯等酯类化合物;此外,烷烃类化合物含量也比较丰富。     

Keggin型缺位杂多酸盐Na_7PW_（11）O_（39）的合成、表征及热稳定性研究

Na2HPO4·12H2O和Na2WO4·2H2O在pH=4.8,恒温358 K的水溶液中反应得到Keggin型缺位杂多酸盐Na7PW11O39.元素分析,红外光谱,紫外光谱,热重-差热分析,原位升温XRD,31P核磁共振等的研究表明：合成样品的分子式为Na7PW11O39.11H2O.     

竹叶椒挥发油成分的研究

研究了竹叶椒挥发油成分。利用水蒸汽蒸馏法提取竹叶椒挥发油，用GC—MS进行分离测定，结合计算机检索技术对分离的化合物进行结构鉴定，应用色谱峰面积归一化法计算各成分的相对百分含量。分离出37个组分，鉴定出32个化学成分，其中含量最高的是苧烯21.76％。     

Noble gas isotopic compositions of deep carbonate rocks from the Tarim Basin

Abundances and isotopic compositions of noble gases (He, Ne, Ar, Kr) with various existence states in carbonate rocks from the Tacan1 Well have been investigated by means of the stepwise heating technique. The elemental abundance patterns of noble gases in the samples show the enrichment of heavy noble gases and depletion of ²⁰Ne relative to the atmosphere, which are designated as type-Ⅰand are similar to that observed in water, natural gases and sedimentary rocks. The ³He/⁴He ratios of deep carbonate samples at lower and medium temperature (300—700℃) and a majority of samples at higher temperature (1100—1500℃) steps are very similar to those of natural gases in the same strata in this area, this feature of radiogenic crustal helium shows that the Tazhong Uplift is relatively stable. However, significant helium and argon isotopic anomalies are found at the 1100℃ step in the Middle-Upper Ordovician carbonate rock, suggesting the incorporation of mantle-derived volatiles, this may be due to minor igneous minerals contained in sedimentary carbonate rocks. The ⁴⁰Ar/ ³⁶Ar ratios in the Cambrian carbonate rock are slightly higher than those in Ordovician carbonate rocks, which may reflect the influence of the chronologic accumulation effect of crust radiogenic ⁴⁰Ar. Argon isotopes of various existence states in source rocks are much more different, both ³⁸Ar/ ³⁶Ar and ⁴⁰Ar/ ³⁶Ar ratios at the higher temperature steps are higher than those at the lower temperature steps.     

塔里木盆地巴麦地区小海子组碳酸盐岩储集层特征与油气成藏

利用岩芯资料,分析巴麦地区小海子组碳酸盐岩储集层特征、影响因素,评价有利储集层分布;应用流体包裹体分析等技术和方法,分析油气藏类型与油气注入成藏史,总结油气成藏规律.研究结果表明:小海子组碳酸盐岩储集层主要岩石类型为颗粒灰岩和白云岩,储集空间类型为孔隙型、孔隙-裂缝型和裂缝型;影响储集层物性的主要因素为沉积作用、成岩作用以及构造作用;最有利的储集层分布区位于巴楚西部巴5-巴参1-麦4-曲1井区一带及周缘;油气藏类型主要为背斜油气藏,其中巴什托背斜油气藏至少发生了海西晚期与喜玛拉雅晚期2次油气注入成藏期,亚松迪Ⅰ号背斜油气藏至少发生了喜玛拉雅晚期1次油气注入成藏期;储集层质量是控制油气成藏的主要因素,构造演化、断裂和圈闭是控制油气成藏的重要因素.     

Discussion on marine source rocks thermal evolvement patterns in the Tarim Basin and Sichuan Basin,west China

Taking marine source rocks of lower Paleozoic in the Tarim Basin and Paleozoic ones in the Sichuan Basin as examples, their sedimentation process could be classified into four styles: continuous subsidence with deep sedimentation in early stage, continuous subsidence with deep sedimentation in later stage, that deeply buried-uplift-shallowly buried, and that shallowly buried-uplift-deeply buried. Unlike that in East China, the marine source rocks evolvement patterns did not accord with sedimentation styles one by one in superimposed basins in west China. Taking local geothermal field into account, four types of source rock evolvement patterns were built: that evolved fast in early stage, evolved fast in middle stage, evolved continuously and evolved in multistage. Among them, the 1st pattern contributed little to the present industrial oil pools directly, but paleo-oil reservoirs and gases cracked from crude oils were main exploration targets. Although some gases were found in the 2nd pattern, the scale was not big enough. For the 3rd and 4th patterns, the hydrocarbon potential depended on organic matters maturity in early stage. For relatively low mature rocks, it was possible to generate some oils in later stage; otherwise the main products were gases. Paleo-oil reservoirs remained fairly well in the Sichuan Basin, and most source rocks underwent kerogen-oil-gas processes, which was useful reference to gas exploration in the Tarim Basin.     

Discussion on marine source rocks thermal evolvement patterns in the Tarim Basin and Sichuan Basin, west China

Taking marine source rocks of lower Paleozoic in the Tarim Basin and Paleozoic ones in the Sichuan Basin as examples, their sedimentation process could be classified into four styles continuous subsldence with deep sedimentation in early stage, continuous subsidence with deep sedimentation in later stage, that deeply buried-uplift-shallowly buried, and that shallowly buried-uplift-deeply buried.Unlike that in East China, the marine source rocks evolvement patterns did not accord with sedimentation styles one by one in superimposed basins in west China. Taking local geothermal field into account, four types of source rock evolvement patterns were built that evolved fast in early stage,evolved fast in middle stage, evolved continuously and evolved in multistage. Among them, the 1st pattern contributed little to the present industrial oil pools directly, but paleo-oil reservoirs and gases cracked from crude oils were main exploration targets. Although some gases were found in the 2nd pattern, the scale was not big enough. For the 3rd and 4th patterns, the hydrocarbon potential depended on organic matters maturity in early stage. For relatively low mature rocks, it was possible to generate some oils in later stage; otherwise the main products were gases. Paleo-oil reservoirs remained fairly well in the Sichuan Basin, and most source rocks underwent kerogen-oil-gas processes,which was useful reference to gas exploration in the Tarim Basin.     

Discussion on marine source rocks thermal evolvement patterns in the Tarim Basin and Sichuan Basin, west China

Taking marine source rocks of lower Paleozoic in the Tarim Basin and Paleozoic ones in the Sichuan Basin as examples, their sedimentation process could be classified into four styles： continuous subsidence with deep sedimentation in early stage, continuous subsidence with deep sedimentation in later stage, that deeply buried-uplift-shallowly buried, and that shallowly buried-uplift-deeply buried. Unlike that in East China, the marine source rocks evolvement patterns did not accord with sedimentation styles one by one in superimposed basins in west China. Taking local geothermal field into account, four types of source rock evolvement patterns were built： that evolved fast in early stage, evolved fast in middle stage, evolved continuously and evolved in multistage. Among them, the 1st pattern contributed little to the present industrial oil pools directly, but paleo-oil reservoirs and gases cracked from crude oils were main exploration targets. Although some gases were found in the 2nd pattern, the scale was not big enough. For the 3rd and 4th patterns, the hydrocarbon potential depended on organic matters maturity in early stage. For relatively low mature rocks, it was possible to generate some oils in later stage; otherwise the main products were gases. Paleo-oil reservoirs remained fairly well in the Sichuan Basin, and most source rocks underwent kerogen-oil-gas processes, which was useful reference to gas exploration in the Tarim Basin.     

哈拉哈塘油田哈6—新垦区块奥陶系碳酸盐岩成岩环境

通过孔洞充填物的碳、氧同位素和包裹体分析,探讨塔里木盆地哈拉哈塘油田哈6—新垦区块奥陶系储层碳酸盐岩的形成环境。除加里东期的淡水喀斯特充填外,还存在海西期埋藏充填、印支—燕山期埋藏充填及喜马拉雅期的埋藏充填。研究表明奥陶系沉积后,经历了同生成岩期、早成岩期和近地表成岩期,后逐步埋藏进入中成岩期,加里东期构造运动使该区经历了抬升、剥蚀以及大气水溶蚀成岩环境,随中生界再次埋藏,构成了中期开启型成岩演化系统。     

Evaluation criteria for gas source rocks of marine carbonate in China

Hydrocarbon generating and expulsion simulation experiments are carried out using samples artifically matched between the acid-dissolved residue of relatively low-maturity limestone and the original sample. This work makes up for the insufficiency of source rock samples with high abundance of organic matters and low maturity in China. The organic carbon content of the 10 prepared samples varies between 0.15% and 0.74%. Pyrolysis data and simulation experiment results of hydrocarbon generating and expulsion, which were obtained by a high-temperature and high-pressure open system, indicate that the lower limit of organic carbon content for marine carbonate rock to generate and expel hydrocarbons is 0.23%—0.31%. In combination with the numerical analysis of organic carbon in marine carbonate rocks from Tarim Basin, Sichuan Basin, Ordos Basin and North China, as well as the contribution of these gas source rocks to the discovered gas pools, we think that the organic carbon criterion for carbonate gas source rocks should be 0.3%.     

Hydrocarbon accumulation in deep fluid modified carbonate rock in the Tarim Basin

The activities of deep fluid are regionalized in the Tarim Basin. By analyzing the REE in core samples and crude oil, carbon isotope of carbon dioxide and inclusion temperature measurement in the west of the Tazhong Uplift in the western Tarim Basin, all the evidence confirms the existence of deep fluid. The deep fluid below the basin floor moved up into the basin through discordogenic fault and volcanicity to cause corrosion and metasomatosis of carbonate rock by exchange of matter and energy. The pore structure and permeability of the carbonate reservoirs were improved, making the carbonate reservoirs an excellent type of deeply buried modification. The fluorite ore belts discovered along the large fault and the volcanic area in the west of the Tazhong Uplift are the outcome of deep fluid action. Such cap bonate reservoirs are the main type of reservoirs in the Tazhong 45 oilfield. The carbonate reservoirs in well YM 7 are improved obviously by thermal fluid dolomitization. The origin and territory of deep fluid are associated with the discordogenic fault and volcanicity in the basin. The discordogenic fault and volcanic area may be the pointer of looking for the deep fluid modified reservoirs. The primary chap acteristics of hydrocarbon accumulation in deep fluid reconstructed carbonate rock are summarized as accumulation near the large fault and volcano passage, late-period hydrocarbon accumulation after volcanic activity, and subtle trap reservoirs controlled by lithology.