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《Analytical letters》2012,45(10):1143-1155
Seeking to improve the quality of cachaça, the Ministério da Agricultura, Pecuária e Abastecimento (Ministry of Agriculture, Livestock and Supply - MAPA), the body responsible for setting and approving regulations governing the Identity and Quality Standards (PIQs) for distilled sugar cane spirits and cachaça, through the Normative Instruction No. 13 of 2005 included some contaminants such as ethyl carbamate (EC), acrolein, lead, and arsenic that must be evaluated in these drinks. Studies on EC, as well as the methods for its determination, are required to evaluate and determine which factors contribute to the formation of this compound in the beverage. An analytical method using gas chromatography/mass spectrometry (GC/MS) with prior sample treatment by solid phase microextraction (SPME) was developed along with the assessment of the principal validation parameters. These two developments lead to the determination of EC with analytical reliability. The optimization of the extraction step was performed via a factorial design involving the selection of parameters such as extraction time, extraction temperature, salt concentration, desorption time, pH, and the method of extraction. The linear range was 5.0 to 200.0 µg L?1 (R2 = 0.9965) with limits of detection and quantification of 1.5 and 5.0 µg L?1, respectively. The recoveries for samples of cachaça containing 10.0 and 80.0 µg L?1 concentrations of EC were 89% and 93%, respectively. The concentrations of EC in the samples of cachaça examined were well below the limits required by Brazilian law. 相似文献
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选择最佳GC/MS分析条件,对工业级和分析级糠醛所含各组分进行分离和检测,通过质谱谱库的计算机检索,结合图谱解析和参考文献定性,鉴定出了十个主要组分。在气相色谱仪上,采用内标法对各组分进行定量,取得了满意的分析结果。 相似文献
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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。 相似文献
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GC-MS联用分析火龙果花提取液的化学成分 总被引:4,自引:0,他引:4
采用GC/MS分析火龙果花无水乙醇、CH2Cl2提取液的化学成分.从无水乙醇和CH2C12提取液中分别分离出60和54个峰,经NIST数据库检索、与标准谱图比较共鉴定出49个化学组分.结果表明,火龙果花中含有维生素E,脂肪酸,烃类和β-谷甾醇、豆甾醇、菜油甾醇等甾醇类化合物. 相似文献
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柴油馏分中含硫化合物组成与分布特征 总被引:2,自引:0,他引:2
采用毛细管气相色谱/脉冲火焰光度检测器(GC/PFPD,Gas Chromatograph/ Pulsed Flame Photometric Detector)对新疆独山子石化公司炼油厂的五种柴油馏分中的硫化物进行了分析。结果表明,常一线馏分中所含的硫化物主要是C0~4苯并噻吩;常二线馏分中除含有C1~4苯并噻吩外还含有大量的C0~3二苯并噻吩及部分未知硫化物;焦化柴油中硫化物组成最为复杂,包含中间馏分油中所有常见的硫化物类型;而催化裂化柴油和加氢柴油中硫化物类型主要为烷基苯并噻吩和烷基二苯并噻吩,其中加氢柴油中的硫化物相对丰度比催化裂化柴油低的多。 相似文献
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C18固相萃取膜适宜处理大体积地下水样现场采样而且易于运输、贮存。利用C18固相膜萃取以及GC/MS联用的方法对地下水中痕量半挥发性有机污染物进行了萃取以及定性、定量分析。优化了固相膜萃取的地下水采样量和浓缩体积。有机氯农药和多环芳烃的平均回收率分别为85%~110.1%、90.3%~115.1%;方法检出限达到10^-9g/L;相对标准偏差均小于15%。本方法用于北京地区地下水中的有机污染物分析,并给出地下水样C18固相膜萃取的GC/MS测定结果。 相似文献
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微波辅助萃取-GC/MS联用分析竹子中氨基酸 总被引:2,自引:0,他引:2
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. 相似文献
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建立和确证了血液中吗啡类毒品(吗啡、 6-单乙酰吗啡、可待因)的液相萃取-硅烷化-GC/MS-SIM检测的方法.以乙基吗啡为内标,以V(CHCl3)∶V(异丙醇)∶V(正庚烷)=50∶17∶33混合溶剂为萃取溶剂,以MSTFA 为硅烷化试剂,采用GC/MS-SIM检测方式,吗啡、6-单乙酰吗啡、可待因的线性相关系数均大于0.99,最低血液检测浓度可达到5 ng/mL;定量范围10~1000 ng/mL;日内重复性小于15%.该方法可用于海洛因吸食者血液中的毒品及其代谢物的检验. 相似文献
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陈晓秋 《分析测试技术与仪器》2005,11(2):123-127
通过有机氮磷农药测定的样品前处理技术一圆盘固相萃取、GC/MS的测定技术—选择离子跳变扫描SIM的应用研究,建立了水体中有机氮磷的分析测定方法.其方法检出限达到了ng/L级的水平。 相似文献
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《Analytical letters》2012,45(15):2311-2317
The present work describes the methodology and validation of gas chromatography with flame ionization (FID) and mass spectrometric (MS) detection after derivatization with N-Methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) for determination of atenolol with an internal standard (metoprolol) in pharmaceutical preparations. The linearity was established over the concentration range of 0.5–20 μg/mL for GC/FID and 12.5–500 ng/mL for GC/MS method. The intra- and inter-day relative standard deviation was less than 4.72 and 5.80%, respectively. Limit of quantification was determined as 500 ng/mL and 12.5 ng/mL for GC/FID and GC/MS, respectively. No interference was found from tablet excipients at the selected assay conditions. Developed GC/FID and GC/MS methods in this study are accurate, sensitive, and precise and can be easily applied to Tensinor tablet as pharmaceutical preparation. 相似文献
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