官厅水库水中莠去津及其降解产物残留的分析

官厅水库拟成为北京市饮用水源,水中的内分泌干扰剂物质也成为重要的监测对象。实验采用MCX固相萃取小柱富集,高效液相色谱法分离,质谱选择离子模式鉴定方法可以同时测定水中痕量除草剂莠去津及其降解产物残留量,检出限可以达到0．02～0．06ug／L,已在北京官厅水库水中检测出莠去津有毒降解产物的残留。其质量浓度在0．155～11．4ug／L,总量在5．97kg(不包括底泥在内)。     

用气相色谱-原子发射光谱法检测VX、Bz及其降解产物

应用气相色谱－原子发射光谱（ＧＣ－ＡＥＤ）同时检测Ｓ－（２－二异丙基氨乙基）甲基硫直膦酸乙酯（ＶＸ）、二苯羟乙酸－３－喹咛环酯（ＢＺ）战剂及其降解产物等５种化合物,得取了Ｃ、Ｈ、Ｓ、Ｎ、Ｏ、Ｐ６种元素色谱图,通过选择合适的检测元素,其检出限ＶＸ为１５．６ｍｇ／Ｌ,Ｂｚ为１６．７９ｍｇ／Ｌ,二异基氨基乙太醇为３．０２ｍｇ／Ｌ,３－羟基喹咛为２８．４０ｍｇ／Ｌ,二苯羟乙酸甲酯为３１．７８ｍｇ／Ｌ,定量     

多杀菌素及其光照降解产物分析

采用五级质谱研究了多杀菌素的质谱断裂规律, 应用串联质谱选择反应检测技术考察了光照条件下多杀菌素的降解程度, 利用液相色谱-质谱联用手段分析了多杀菌素降解产物, 并推断了主要降解产物的结构. 结果表明, 多杀菌素17碳上的福乐糖胺容易失去, 三氧甲基鼠李糖很稳定; 多杀菌素浓度随紫外光照射时间的增加而降低, 在照射484 min后, 降解率达到70%左右, 形成11种降解产物, 这些降解产物是多杀菌素A或D经氧化、还原及水解等反应形成.     

肉桂醛催化加氢产物的GC-MS分析

肉桂醛(1)是α、β不饱和羰基化合物中具有代表性的一种物质,其加氢过程如下所示:     

异松油烯空气氧化产物的GC-MS分析

用气相色谱-质谱联用技术对异松油烯的空气氧化产物进行了分析,确定其主要产物为p-伞花醇、p,α-二甲基苯乙烯、对伞花烃、双戊烯等,并通过改变温度、溶剂等对氧化产物中各成分的含量变化进行了研究.     

GC-MS检测大鼠尿液中曲马多及其代谢产物

曲马多为中枢作用的阿片类镇痛药物,为非选择性的μ,δ和κ阿片受体激动剂,通过抑制神经元突触对去甲肾上腺素的再摄取,增加神经元外5-羟色胺浓度,影响痛觉传递而产生镇痛作用;因此适用于中度至重度疼痛,如晚期癌症病人,也常用于阿片依赖患者镇痛,但长期服用可形成对盐酸曲马多的依赖,可产生阿片类药物戒断及中毒症状[1-2].     

活性白土催化松香反应产物的GC-MS分析

把活性白土上松香催化反应产物分离为酸性物和中性物,采用气相色谱-质谱联用技术(GC-MS)分别对各部分化学组成进行定性定量分析.结果表明,活性白土上松香主要进行脱氢、脱羧及裂解反应,其产物中的酸性物共分离出2个峰,主要成分是脱氢枞酸,含量为99.61%;中性物共分离出35个峰,初步鉴定出其中33个组分,大部分为甾族类化合物和环烯烃类化合物,主要成分是5α-雄甾烷、1,4-二甲基-7-(1-甲基乙烯基)-1,2,3,5,6,7,8,8a-八氢化-1S-(1α)-蓝烃、松香酸甲酯和(-)-石竹烯,含量分别为18.75%、13.00%、12.53%和11.74%.     

LC-ESI-MS分析两性霉素B降解产物

两性霉素B(amphotericinB)是一种常用的抗真菌抗生素,属于多烯大环内酯类化合物,化学性质不稳定,在生产和储存过程中容易发生多种降解反应,产生无活性甚至有毒性的降解物,直接影响产品质量和临床用药的安全,因此,研究该抗生素降解物和降解途径,对防止产品降解、保证产品质量非常必要。已有不少有关两性霉素B各种剂型稳定性的研究报道,ThomaK等研究报道了多烯类抗生素光稳定性结果,然而有关两性霉素B在酸、碱、加热、氧化和光照等条件下降解途径研究未见报道。由于直接分离鉴定各降解产物比较困难,本实验采用LC-MS在线分析手段,直接分析检测降解产物。实验表明,通过检测各种加速实验样品的降解物,可以确立降解途径和降解物,本文对控制降解反应发生、提高产品质量以及稳定性研究具有重要意义。     

广藿香超临界CO_2萃取产物的GC-MS分析

采用超临界CO2 流体萃取技术从广藿香中提取出挥发油 ,挥发油得率为2.97 %(w)。采用GC -MS分离鉴定其化学组成 ,以面积归一化法测定其相对含量。从广藿香叶挥发油中鉴定出24个化合物 ,其中以广藿香醇 (48.8 % )、δ_愈创木烯 (15.2 % )、α_愈创木烯(15.3 %)等为主     

原油与沥青质热解产物的GC-MS分析

较严重生物降解的原油没有正构烷烃,甚至缺失类异二戊烯烃,给油源研究造成一定困难.这种降解油中沥青质含量很高,用沥青质热解可产生相当量的正构烷烃和其它的烃类成分,例如:类异戊二烯烃、甾烷、萜烷、芳烃等成分也会有所变化.本文研究它们的变化特点、变化的幅度,找出一定的规律性,以对利用原油沥青质热降解产物用于油源对比时分析它们的相似性有所帮助.实验证明,总体上看沥青质的热降解产物与原油的烃类分布上比较相似,但并不一致,有的差距比较大,应该做一些校正,有的则比较稳定可靠.     

水产品中酰胺类除草剂及其代谢物的气相色谱-质谱法测定

建立了同时测定水产品中5种酰胺类除草剂(乙草胺、甲草胺、异丙甲草胺、丁草胺、丙草胺)及其代谢物2-甲基-6-乙基苯胺(MEA)、2,6-二乙基苯胺(DEA)的气相色谱-质谱联用(GC-MS)分析方法.样品经二氯甲烷-乙酸乙酯(3:2,体积比)混合溶剂提取,正己烷洗脱后进行GC-MS检测.在优化检测条件下,MEA、DEA...     

Reactions of VX, GB, GD, and HD with nanosize Al(2)O(3). Formation of aluminophosphonates.

Room-temperature reactions of VX, GB, GD, and HD with nanosize Al(2)O(3) (AP-Al(2)O(3)) have been characterized by (31)P, (13)C, and (27)Al MAS NMR. Nerve agents VX, GB, and GD hydrolyze to yield surface-bound complexes of their corresponding nontoxic phosphonates. At sufficiently high loadings, discreet aluminophosphonate complexes, Al[OP(O)(CH(3))OR](3), are generated which are identical to synthesized model compounds. Thus the reaction with phosphonic acids is not just surface-limited, but can continue to the core of alumina particles. HD mainly hydrolyzes at lower loadings to yield thiodiglycol (TG, 71%) and a minor amount of the CH-TG sulfonium ion (12%), although some elimination of HCl is also observed (17%). The reactive capacity for HD is evidently exceeded at high loadings, where complete conversion to TG is hindered. However, addition of excess water results in the quantitative hydrolysis of sorbed HD to CH-TG. On AP-Al(2)O(3) dried to remove physisorbed water, (13)C CP-MAS NMR detects a surface alkoxide consistent with that of TG.     

气相色谱-质谱法测定纺织材料及制品中16种限用有机锡类化合物

采用气相色谱-质谱(GC-MS)技术建立了纺织材料及其制品中16种限用有机锡类化合物的测定方法。以甲醇和乙酸钠的混合溶液作为提取剂,对样品进行超声提取,提取液经四乙基硼酸钠衍生化后,再用正己烷进行萃取,DB-5MS(30 m×0.25 mm×0.25μm)色谱柱分离,气相色谱-质谱选择离子模式进行分析检测,内标法定量。16种有机锡类化合物在50~500μg/L质量浓度范围内与峰面积呈线性关系,方法的定量下限均为0.05 mg/L(0.15 mg/kg)。样品加标回收率为77.6%~106.0%,相对标准偏差(RSD,n=6)不大于8.3%。结果表明该方法快速可靠、准确简便,适用于纺织材料及制品中有机锡类化合物的分析检测。     

Decontamination of VX, GD, and HD on a surface using modified vaporized hydrogen peroxide

Vaporized hydrogen peroxide (VHP) has proven efficacy for biological decontamination and is a common gaseous sterilant widely used by industry. Regarding chemical warfare agent decontamination, VHP is also effective against HD and VX, but not GD. Simple addition of ammonia gas to VHP affords reactivity toward GD, while maintaining efficacy for HD (and bioagents) and further enhancing efficacy for VX. Thus, modified VHP is a broad-spectrum CB decontaminant suitable for fumigant-type decontamination scenarios, i.e., building, aircraft, and vehicle interiors and sensitive equipment. Finally, as an interesting aside to the current study, commercial ammonia-containing cleaners are also shown to be effective surface decontaminants for GD, but not for VX or HD.     

二环己胺中微量苯胺等杂质的气相色谱与气-质联用分析

二环己胺可由苯胺催化加氢制得,故产物中有苯胺等杂质存在。苯胺等杂质对二环己胺产品质量有严重的影响,因此二环己胺纯度需达到99．5％以上,苯胺的含量应低于0．1％。本文以苯甲醇为内标,建立了二环己胺产品中微量苯胺的气相色谱分析条件,并且采用气相色谱一质谱(GCMS)分析了各杂质峰的归属,发现二环己胺产品纯度达不到     

染毒水样中神经性毒剂水解产物的分析

考察了对水中6种神经性毒剂水解产物固相萃取的萃取剂,洗脱剂等因素对萃取率的影响,以LC－CN小柱为萃取剂,1％冰醋 甲醇溶液为洗脱剂,测得萃取回收率为59．7％－100％,相对标准偏差为1．4％－7．2％,采用气相色谱和色质联用－选择离子检测法对水解产物三甲基硅烷（TMS）衍生物进行分析鉴定,水中水解产物最低检测浓度为0．002－0．02mg/L。为今后水中神经性毒剂未知样品分析提供了简便,快速的分析方法。     

气相色谱-质谱法对水中亚磷酸三乙酯测定方法研究

亚磷酸三乙酯是生产有机磷神经毒剂的中间体,属于"禁止化学武器公约"的化学品.它同时是一种重要的染料中间体,广泛应用于造纸、染料、医药、化工、农药等行业中.     

Quantification of Transformation Products of Unsymmetrical Dimethylhydrazine in Water Using SPME and GC-MS

Quantification of trace concentrations of transformation products of rocket fuel unsymmetrical dimethylhydrazine (UDMH) in water requires complex analytical instrumentation and tedious sample preparation. The goal of this research was to develop a simple and automated method for sensitive quantification of UDMH transformation products in water using headspace (HS) solid-phase microextraction (SPME) in combination with GC-MS and GC-MS/MS. HS SPME is based on extraction of analytes from a gas phase above samples by a micro polymer coating followed by a thermal desorption of analytes in a GC inlet. Extraction by 85 µm Carboxen/polydimethylsiloxane fiber at 50 °C during 60 min provides the best combination of sensitivity and precision. Tandem mass spectrometric detection with positive chemical ionization improves method accuracy and selectivity. Detection limits of twelve analytes by GC-MS/MS with chemical ionization are about 10 ng L^?1. GC-MS provides similar detection limits for five studied analytes; however, the list of analytes detected by this method can be further expanded. Accuracies determined by GC-MS were in the range of 75–125% for six analytes. Compared to other available methods based on non-SPME sample preparation approaches (e.g., liquid–liquid and solid-phase extraction), the developed method is simpler, automated and provides lower detection limits. It covers more UDMH transformation products than available SPME-based methods. The list of analytes could be further expanded if new standards become available. The developed method is recommended for assessing water quality in the territories affected by space activities and other related studies.