水性涂料VOG的气相色谱-质谱检测前处理方法研究

对水性涂料挥发性有机化合物（VOC）检测的前处理方法进行了研究.分别采用搅拌萃取法和超声波萃取法对水性涂料中28种VOC进行提取,采用离心方法提取清液,采用气相色谱-质谱法测定并计算回收率.通过比较,确定以二氯甲烷为萃取溶剂、搅拌时间为40 min的搅拌萃取法提取效率更高,采用该方法对28种VOC的加标回收率在94％～116％之间.     

HS-SPME结合GC-MS分析煎鸡蛋的挥发性风味成分

采用顶空固相微萃取与GC-MS联用方法对煎鸡蛋中挥发性成分进行提取与分析,考察萃取头、萃取温度和吸附时间对分析结果的影响,得到优化的顶空固相微萃取条件为:黑色萃取头(75μm Carboxen/PDMS),吸附温度75℃,吸附时间70 min。在优化的条件下分析,共鉴定出50种挥发性风味成分,其中,醛类16种(40.588%)、含氮化合物14种(23.639%)、醇类8种(7.156%)、烃类3种(4.800%)、酚类及杂环化合物3种(1.755%)、酮类3种(0.868%)及含硫化合物3种(0.563%)。鉴定出含量较高(相对质量分数大于2.5%)的物质有:2,5-二甲基吡嗪、3-甲基丁醛、2-甲基吡嗪、壬醛、苯甲醛、反,反-2,4-癸二烯醛、辛醛、2-甲基丁醛、反-2-癸烯醛、3,7-二甲基-1,6-辛二烯、1-辛烯-3-醇。     

臭荚蒾挥发性成分分析

采用水蒸气蒸馏法提取臭荚蒾中的挥发油,经GC/MS分析,从臭荚蒾挥发油中分析鉴定出了28个挥发性成分,占挥发油总量的95.6%。化合物类型包括倍半萜、酚类化合物和脂肪族等,其中酚类化合物的含量最高,占挥发油总量的86.03%。主要成分为丙烯酚(64.98%),其次为乙酰丁香油酚(12.52%)、丁香油酚(7.80%)和冬青油(5.10%)。     

三七挥发性物质的气相色谱分析

本项目利用气相色谱-质谱联用仪对中药三七蒸汽溶液进行分析研究,建立了相应的测定方法及获得相应的气相色谱图谱。通过检索美国国家标准与技术局(NIST)的质谱图库,测得了19种可能化合物,其中2-甲氧基-4-(1-丙烯基)-苯酚、十四烷酸、十八碳二烯酸、二十五烷的可信度达95%以上。     

便携式GC-MS在应急监测中的应用

随着我国经济的高速发展,企业生产的不断扩张,企业的环境突发事故的多变性,对现场监测提出了更高的要求。建立便携式GC-MS,由于其体积小,分析精度高,非常适合于现场挥发性有机物的分析,在国内已被成功用于多起现场环境应急监测工作,本文以一次监测实例说明通过充分利用该仪器快速检测极低浓度挥发性有机污染物的功能,可将之进一步应用于被污染环境空气的实时现场监测,从而为复杂情况下环境污染源的快速排查工作提供强有力的技术支持。     

不同产地烟草精油的提取及化学组成分析

选取四川、贵州和福建三地烟草为原料,用水中蒸馏法提取烟草精油。采用气相色谱-质谱联用(GC-MS)仪对不同产地烟草精油的组成及含量进行分析,比较了不同产地对产物产率及组成的影响。研究结果表明:产自福建、四川和贵州的烟草平均得率分别为0.1391%、0.0851%和0.1075%,相应的新植二烯分别为39.86%、36.12%和44.88%。对比分析显示:产自福建的烟草得油率最高,特征香气适中;产自贵州的烟草精油得油率适中,烟草香气突出,有明显甘草香气;产自四川的烟草精油得油率较低,香气较弱。     

Research on the relationship between cephalosporin structure,solution clarity,and rubber closure compatibility using volatile components profile of butyl rubber closures

Objective: Establish an effective experimental strategy to determine the compatibility of rubber closures for drugs.

Significance: Various types of rubber closures with different compositions are available for drug packaging. Many additives of rubber closures can be released from rubber closures and may affect the quality of drugs and pose a risk to human health. In this study, we aimed to determine the relationship between cephalosporin structure, solution clarity, and rubber closure compatibility using volatile components profile of butyl rubber closures.

Methods: Two opposite polarity gas chromatography (GC) systems and GC-mass spectrometry (MS) were used to achieve rapid qualitative determination of the main volatile components in rubber closures. Simulated adsorption experiment was performed to investigate the adsorption of main volatile components in rubber closures by cephalosporins with different side chain structures, and to determine the effects of adsorption on solution clarity.

Results: A volatile components screening library of rubber closures was established and the structures of some volatile component were confirmed. The specific adsorption of the structure of cephalosporins on volatile components from rubber closures was studied.

Conclusion: Based on the results of this study, rubber closures with good compatibility for cephalosporins with different side chain structures can be selected rapidly. This experimental strategy not only facilitates the screening of suitable rubber closures more effectively, but also enables the quick determination of volatile components adsorbed by drugs.     

茶叶中多种氨基酸15N同位素丰度的检测研究

建立了气相色谱-质谱联用（GC-MS）测定茶叶中丙氨酸、丝氨酸、谷氨酸、天冬酰胺、茶氨酸、谷氨酰胺氨基酸同位素丰度的检测方法。茶叶样品经浸泡提取后，经N-甲基-N-（三甲基硅烷）三氟乙酰胺（MSTFA）进行衍生，在优化的色谱-质谱条件下，6种目标氨基酸衍生物均检出。验证了丙氨酸、丝氨酸、谷氨酸、天冬酰胺、茶氨酸、谷氨酰胺的¹⁵N同位素丰度在10%~98%内均可以被准确测定。建立的方法精密度优于0.6%，绝对偏差小于0.6%。所建立的方法样品前处理简单，同位素丰度检测准确，可满足茶叶中标记氨基酸同位素丰度检测，该方法也可推广至不同农作物中氨基酸同位素丰度的检测，为植物中氨基酸相关转化路径及代谢循环研究提供技术支持。     

Spatio-temporal variability in the fatty acid profile of the adductor muscle of the common cockle Cerastoderma edule and its relevance for tracing geographic origin

The present study aimed to identify the potential existence of spatio-temporal variability in the fatty acid (FA) profile of the adductor muscle (AM) of a commercially important bivalve, the common cockle Cerastoderma edule, and determine if such variability can be used to trace their geographic origin post-harvesting. Common cockles were sampled in eight ecosystems along the coast of mainland Portugal, as well as in two different channels within one of those ecosystems over two consecutive years. Results showed significant differences in FA profiles among ecosystems, namely due to different levels of eicosapentaenoic acid (EPA; 20:5n-3), arachidonic acid (20:4n-6), ratio of polyunsaturated FA (PUFA) n-3/n-6, monounsaturated FA (MUFA; 18:1n-9 and 20:1n-9/11) and bacterial FA (15:0, 17:0 and 18:1n-7). FA profiles also displayed significant differences between two consecutive years in channels from the same ecosystem. Overall, while the FA profile displayed by the AM of C. edule can be successfully used to trace their geographic origin, the existence of temporal variability requires a periodical verification of FA signatures to identify potential shifts, namely when comparing specimens from the same ecosystem.