对2008年一道高考化学题的实验研究——是对甲基苯酚还是邻甲基苯酚

2008年一道高考化学题曾引起过不小的争论。争论的焦点是,一种甲基苯酚,与溴水反应生成的一溴代物只有2种,它应该是对甲基苯酚还是邻甲基苯酚?为了解决上述问题,用GC/MS法进行了实验研究。结果表明：对甲基苯酚与溴水反应生成的一溴代物只能观察到1种,而邻甲基苯酚与溴水反应生成的一溴代物则能观察到2种,二者均未观察到生成羟基间位溴代产物。由此可得出结论,该化合物应该是邻甲基苯酚。     

调味品中氯丙醇的GC/ECD和GC/MS/MS衍生化检测方法研究及应用

报道了调味品中氯丙醇的衍生化气相色谱(GC／ECD)和衍生化气相色谱双串联质谱法(GC／MS／MS)测定。GC／ECD测定酱油中3—氯—1，2—丙二醇(3—MCPD)的检出限达到0．01mg／kg，回收率为91％～104％，变异系数为2．27％～7．96％；GC／MS／MS同时测定酱油中1，3—二氯—2—丙醇、2，3—二氯—1—丙醇和3—氯—1，2—丙二醇，1，3—二氯—2—丙醇、2，3—二氯—1—丙醇的检出限为0．02mg／kg，3—氯—1，2—丙二醇的检出限为0．01mg／kg，回收率在92％～106％，变异系数为3．51％～13．33％。     

GC/MS测定锅巴中丙烯酰胺含量

建立了一种测定市售锅巴中的丙烯酰胺含量的方法.该法样品前处理不必经过溴化衍生,样品脱脂后用水提取丙烯酰胺,提取液过活性炭柱,再用乙酸乙酯将活性炭柱中吸附的丙烯酰胺洗脱.洗脱液浓缩后经气相色谱-质谱(GC-MS)定量分析,检测限为0.06 mg/kg,适合测定市售锅巴中的丙烯酰胺的含量.还考察了丙烯酰胺在水的固液两相中的分配比.     

固相微萃取-气相色谱-质谱法测定纤维制品中游离甲醛

本文建立了纤维制品中游离甲醛的固相萃取-气质联用测定方法。试样剪碎后置于饱和NaCl溶液中60℃超声处理30 min,经五氟苯盐酸羟胺(PFBOA)衍生化后,采用顶空固相微萃取和色质联用技术(HS-SPME-GC/MS),选择离子(m/z181)进行定量。该方法适用于各类单层或多层纤维织物中甲醛的测定,加标回收率分别为94.9%~98.7%,相对标准偏差(RSD)在2.97%~4.59%之间,检出限为0.02 mg/kg。     

GC/MS方法分析豇豆中水胺硫磷等37种农药残留

建立了GC/MS法同时测定豇豆中水胺硫磷等37种农药残留的方法.农药经过乙腈提取,NH2/CARBON复合固相萃取小柱净化,HP-5MS(30 m×0.25 mm×0.25 μm)弹性石英毛细管柱分离后,用GC/MS选择离子模式进行测定.农药在0.020～0.500 mg/L时与峰面积有良好的线性关系(r2>0.990...     

微波辅助萃取-GC/MS联用分析竹子中氨基酸

建立了微波辅助萃取-GC/MS联用测定竹子中谷氨酸、天冬氨酸和苯丙氨酸等10种氨基酸的分析方法, 优化了微波辅助萃取条件, 方法的线性范围在0.100～100 μg/mL之间, 检出限在0.0098～0.36 μg/mL之间, RSD为4.1%～9.7%, 回收率在84.3%～118%之间. 分析了4种不同产地、竹龄竹子的竹叶、竹枝和竹沥中氨基酸含量. 结果表明, 不同竹种、产地及竹龄的竹子中氨基酸总量有较大差异;相同竹种其竹沥中氨基酸含量显著高于竹叶及竹枝中氨基酸含量.     

Identification of arsenolipids with GC/MS

Arsenic-containing hydrocarbons have recently been reported as natural constituents of fish oil. We report a simple method for determining these compounds by GC/MS. Application of the methodology will delineate the distribution of these novel arsenic compounds in foods, and facilitate an assessment of the toxicological implications.     

烟草制品中紫苏葶的气相色谱/质谱法分析

以二氯甲烷为溶剂,丙酸苯乙酯为内标,将烟草制品进行萃取,经固相萃取柱纯化,采用气相色谱／质谱法定量分析了烟草制品中的紫苏葶．方法的定性检测限为0．11μ/g,定量检测限为0．36μ/g,平均回收率为95．53％,相对标准偏差（RSD）为1．89％．     

基于GC/Q-TOF MS技术鉴定S-zorb汽油中噻吩类化合物

结合气相色谱分离技术和MS/MS串联质谱筛查技术,通过选定目标母离子进行碰撞诱导解离,获取精确质量子离子信息,实现汽油馏分中噻吩类化合物的痕量筛查分析.选取5种不同碳数取代噻吩类化合物作为标准物绘制定量标准曲线,建立了基于气相色谱-四极杆串联飞行时间质谱(GC/Q-TOF MS)直接测定汽油中噻吩类化合物的方法.利用该...     

气相色谱-质谱联用分析2-氯-5-三氯甲基吡啶

2-氯-5-三氯甲基吡啶是重要的农药中间体.采用气相色谱-质谱联用法,对高效除草剂盖草能的中间体2-氯-5-三氯甲基吡啶的分析条件进行了探讨和优化.使用Rts-5MS毛细管柱,EI电离源,实验结果的线性关系良好,相关系数r=0.9921,回收率为99.05%,相对标准偏差为0.78%.     

GC/MS法测定大米中精噁唑禾草灵和氰氟草酯残留量

采用乙腈提取,NH2固相萃取柱净化,GC/MS测定,建立了大米中精噁唑禾草灵和氰氟草酯残留量的测定方法。添加精噁唑禾草灵质量分数为0.02,0.2,0.5mg/kg,平均回收率分别为82.3%,88.8%和90.7%,相对标准偏差分别为6.8%,8.2%和3.7%,检出限为0.02 mg/kg;添加氰氟草酯质量分数为0.02,0.2,0.5mg/kg,平均回收率分别为87.7%,94.2%和92.3%,相对标准偏差分别为8.6%,5.6%和7.3%,检出限为0.02mg/kg。     

Differentiation and dating of red ink entries of seals on documents by HPLC and GC/MS

A novel approach for differentiation and dating of red ink entries of seals on documents was developed based on ion‐pairing HPLC (IP‐HPLC) and GC/MS. Sixty‐nine red ink pastes of seals were collected and the chromatographic conditions for separation of the dye components by IP‐HPLC and the volatile additives by GC/MS in the ink entries were optimized. According to the dye components and additives, the ink entries were classified by HPLC with a multi‐wavelength UV detector. The volatile components of the inks were identified by GC/MS and the classification of the ink entries was also investigated based on these volatile additives. The results showed that most of the ink entries of the seals can be differentiated by combining HPLC with a multi‐wavelength detector and GC/MS methods. The degradation of the standard dye mixtures and the compositional changes of the ink entries of seals were investigated in light or natural aging conditions. The results indicated that the dye components decomposed in light or natural storage conditions, while the rates of the degradation depended on the structures of the dye components, the aging conditions, even the additives of the ink pastes. The results also showed that there existed good relationships between the compositional changes of the ink entries and the aging time, which can provide scientific evidences and valuable clues for dating of the ink entries.     

化妆品中碘丙炔醇丁基氨甲酸酯的高效液相色谱检测及质谱确证

建立了高效液相色谱(HPLC)-二极管阵列检测器(DAD)测定化妆品中碘丙炔醇丁基氨甲酸酯的方法.化妆品样品经超声提取后,高效液相色谱-二极管阵列扫描检测,并在235 nm波长进行分析.用保留时间结合紫外光谱定性,外标法定量,并采用液相色谱-质谱法确证.碘丙炔醇丁基氨甲酸酯的回收率为92.7%～99.8%,相对标准偏差在0.8%～2.1%之间,定量限为20 mg/kg.     

硒芳香杂环化合物的GC/MS分析

本文对合成的7种含硒芳香杂环化合物进行了GC／MS分析研究。结果表明：BS、MB、BBS和DBBS等4个化合物在色谱柱内的保留时间与它们的相对分子质量呈线性关系。所有化合物均可获得特征质谱,表现出含单个硒原子的分子离子或碎片离子特征峰簇,硒的两种主要同位素在峰簇中表现为主要峰M与（M-2）的相对丰度比约为2：1,可为鉴定含硒分子离子或碎片离子提供重要信息。新化合物1,2,5-硒二唑并[3,4-d]嘧啶-5,7-（4H,6H）二酮（SPDO）在色谱柱内出现11．83min和7．96min两个具有相同的质谱的色谱峰,被认为是互变异构体的峰。     

Determination of Aroma Compounds in Blackberry by GC/MS Analysis

The aromatic composition of five blackberry cultivars (Bursa 2, Navaho, Nessy, Chester Thornless, and Jumbo) was studied. The Im-SPME (Immersion Solid Phase Micro Extraction) extraction technique was applied and the samples were analyzed by GC/MS. Furfural and its derivatives were found to be the major aromatic compounds and 5-hydroxymethylfurfural was the most abundant compound in all the blackberry varieties.     

Analysis of anabolic steroids in hair by GC/MS/MS

A simple and sensitive gas chromatography/tandem mass spectrometry (GC/MS/MS) method is described for the detection of anabolic steroids, usually found in keratin matrix at very low concentrations. Hair samples from seven athletes who spontaneously reported their abuse of anabolic steroids, and in a single case cocaine, were analyzed for methyltestosterone, nandrolone, boldenone, fluoxymesterolone, cocaine and its metabolite benzoylecgonine. Anabolic steroids were determinate by digestion of hair samples in 1 m NaOH for 15 min at 95 degrees C. After cooling, samples were purificated by solid-phase and liquid-liquid extraction, then anabolic steroids were converted to their trimethylsilyl derivative and finally analyzed by GC/MS/MS. For detection of cocaine and benzoylecgonine, hair samples were extracted with methanol in an ultrasonic bath for 2 h at 56 degrees C then overnight in a thermostatic bath at the same temperature. After the incubation, methanol was evaporated to dryness, and benzoylecgonine was converted to its trimethylsilyl derivative prior of GC/MS/MS analysis. Results obtained are in agreement with the athletes' reports, confirming that hair is a valid biological matrix to establish long-term intake of drugs.     

采用配备GPC纯化装置的GC/MS进行农产品中农药残留的快速分析

本文采用GPC-GC／MS在线连接系统和固相萃取的方法快速测定农产品中的农药残留。该方法首先用液-液分配法从均化的食物样品中提取农药,然后用PSA结合相进行固相萃取,最后进行GPC-GC／MS分析。GPC-GC／MS系统包括一套GPC净化装置,可以简化样品前处理步骤。把浓度为0．1 μg／g的97种农药添加到马铃薯、甘蓝和胡萝卜中,得到了比较好的回收率。整个分析过程大约需要50 min。     

毛细管色谱-质谱法测定环境大气中挥发性有机污染物

毛细管色谱-质谱法测定了环境大气中挥发性污染物。用液氧冷冻法和常温吸附法(TenaxGC)分别采集大气样品,然后用两种系统进行浓缩,并进入毛细管色谱-质谱体系,完成了有机污染物的定性定量分析。解决了一些色谱-质谱联用中的问题。并且还讨论了无分流进样问题,比较了两种采样方法。用此方法测定了某炼油厂环境大气中的污染物。