顶空-气相色谱/质谱联用法检测食品添加剂中的甲醇

建立了一种快速准确的顶空-气相色谱/质谱联用检测食品添加剂中甲醇含量的方法。该方法选择去离子水作为顶空基质校正剂,样品检测不需要过多前处理,操作简便快捷,甲醇标准工作曲线的相关系数大于0.9990,方法检出限和定量限分别为0.80mg/kg和2.67mg/kg,实际样品的加标回收率范围为96.37%～99.95%。结果表明,该方法可实现食品添加剂中甲醇的快速准确测定。     

紫藤鲜花香气化学成分的研究

采用固相微萃取吸附采集紫藤(Wistariasinensis)花的香气成分,用色谱/质谱联用分析鉴定,并用GC/MS总离子流色谱峰的峰面积进行归一化定量分析紫藤鲜花的香气成分,鉴定出2十一酮21.22%、2壬酮20.09%、3[4,8二甲基3,7壬二烯]呋喃10.32%、2十三酮8.21%、芳樟醇7.5%、β石竹烯6.02%、反式罗勒烯5.41%、草蒿脑4.27%、反式茴香脑3.91%、反,反2,4辛二烯1醇乙酸酯1.65%、α蒎烯氧化物1.32%、2十五酮1.14%、大根香叶烯D1.14%和4丙酮基环庚酮1.11%等32种化合物。固相微萃取气相色谱/质谱法是一种可用于鲜花香气成分分析的简单可行的分析方法。     

固相微萃取-气相色谱串联两级质谱法测定水中10种藻类代谢产物

文中建立了固相微萃取-气相色谱串联两级质谱法测定地表水中的10种藻类代谢产物的含量,研究了萃取时间、萃取温度、萃取剂量、萃取纤维等预处理参数对嗅味物质含量的影响,同时对不同规格的色谱柱进行分离效果比较。结果表明,在萃取时间为25 min、萃取温度为65℃、氯化钠含量为1.7 g的测定条件下,采用50/30μm DVB/CAR/PDMS萃取头进行预处理,HP-5MS色谱柱进行分离,质谱检测器进行测定,可以使检测结果达到最优效果。方法的质量浓度均达到5.00～100.00 ng/L,工作曲线回归方程的相关系数R²>0.995;方法检出限(2S/N)为0.14～1.00 ng/L。在纯水加标量为20.00、50.00、80.00 ng/L时,平均回收率为92.0%～109.0%,精密度RSD为0.4%～8.9%,实际水样加标的平均回收率为83.9%～101.8%。该方法检测浓度数量级在纳克级,灵敏度较固相萃取-气相色谱-质谱法提高1 000倍,更适合地表水和饮用水中低浓度藻类代谢产物的检测要求。     

丙环唑土壤降解影响因素研究

建立了高效液相色谱串联质谱(LC-MS/MS)检测土壤中丙环唑的方法。采用室内模拟实验,对不同土壤及含水率、微生物、有机质和pH等因素对丙环唑降解的影响进行了研究。结果表明:土壤中有机质和微生物不是丙环唑在土壤中降解的主要影响因子。含水率和pH对丙环唑的降解产生显著影响,土壤的含水率越高,pH越小,土壤中丙环唑的降解越快。丙环唑在土壤中的降解主要受pH的影响。     

The Thermal Degradation of Some Polymers Based Upon p-Hydroxybenzoic Acid

Three polymers based upon p-hydroxybenzoic acid have been studied by thermogravimetry to ascertain their relative thermal stabilities in both inert and oxidising atmospheres. Experiments have been carried out at a rate of temperature rise of 2°C min^?1 and isothermally at a number of temperatures. The polymers have good thermal stability. They have also been examined by pyrolysis gas chromatography mass spectrometry using two different procedures. In the first, fresh samples were pyrolysed at a number of increasing temperatures, whereas in the second, the same sample was subjected to successive pyrolyses at the same temperature intervals. The results are compared with those of other authors derived using different techniques.     

用气相色谱-质谱法分析液化石油气和液化天然气中的硫化合物含量

研究了用气相色谱 -质谱联用测定天然气中硫化合物 ,分析了从不同油田收集的天然气样品 ,所得结果精密度及准确度良好 ,每种硫化合物的检测极限都在 1× 10 -6之下 (质量比 )     

福建省水产动物苗种中氯霉素残留现状研究

对2008-2011年4年中对福建省内各种苗孵化基地随机抽检的17个经济苗种共计204个批次的样品,采用高效液相色谱-串联质谱联用法检测氯霉素含量。结果显示:大黄鱼,对虾中检出率较高。     

Lipidomics by Supercritical Fluid Chromatography

This review enlightens the role of supercritical fluid chromatography (SFC) in the field of lipid analysis. SFC has been popular in the late 1980s and 1990s before almost disappearing due to the commercial success of liquid chromatography (LC). It is only 20 years later that a regain of interest appeared when new commercial instruments were introduced. As SFC is fully compatible with the injection of extracts in pure organic solvent, this technique is perfectly suitable for lipid analysis and can be coupled with either highly universal (UV or evaporative light scattering) or highly specific (mass spectrometry) detection methods. A short history of the use of supercritical fluids as mobile phase for the separation oflipids will be introduced first. Then, the advantages and drawbacks of SFC are discussed for each class of lipids (fatty acyls, glycerolipids, glycerophospholipids, sphingolipids, sterols, prenols, polyketides) defined by the LIPID MAPS consortium.     

The Separation and Identification of Higher Molecular Weight Fullerenes

A nonaqueous, reversed-phase separation of the fullerenes is described. The bonded-phase, a polymeric octadecyl one, has previously been shown to have a very large separating power for nonplanar polycyclic aromatic hydrocarbons. This work shows that this shape selectivity also is found with the fullerenes, allowing very short retention times while maintaining separation of the C₆₀ and C₇₀ species. Additionally, a fraction containing larger fullerenes was isolated. UV absorbance spectra of these species were obtained. Preliminary spectra of hydrogen chemical ionization mass spectra were also obtained and showed that the fullerenes adsorb large amounts of molecular hydrogen.     

促传剂强化臭氧氧化对硝基酚的研究

研究了传质促进剂（促传剂）对臭氧降解水中对硝基酚的影响，筛选出了两种效果较好的促进剂。实验测定了臭氧在鼓泡反应塔中的传质系数以及添加促传剂后传质系数增大的倍数。还测定了添加促传剂后酚溶液表面张力的变化，并初步探讨了促传剂的作用机理。     

食品中野燕枯残留量的测定

建立了气相色谱-质谱选择离子法（GC-MSD）测定食品中野燕枯残留量的检测方法。试样用水．丙酮（体积比为1：4）振荡提取,经二氯甲烷液-液分配,以凝胶色谱柱净化,再经氟罗里硅土（Florisil）固相柱净化。洗脱液浓缩并溶解定容后,供气相色谱,质谱仪检测,外标法定量。回收率范围为84．5％。98．0％;相对标准偏差为3．19％-6．74％;测定低限为0．010mg／kg。     

POLYCYCLIC AROMATIC HYDROCARBON REFERENCE RANGE LEVELS IN THE U.S. POPULATION BY MEASUREMENT OF URINARY MONOHYDROXY METABOLITES

We developed a gas chromatography/isotope dilution high- resolution mass spectrometry (GC/ID-HRMS) method for measuring 18 PAH metabolites representing 8 parent PAHs in 3 mL of urine at low part-per-trillion levels. We applied this method to the analysis of urine specimens from approximately 2400 people who participated in the National Health and Nutrition Examination Survey for the years 1999 and 2000 to determine levels for 14 PAH hydroxy metabolites of 7 parent compounds. Using this GC/ID-HRMS method, we found detectable concentrations for monohydroxy metabolite isomers of fluorene, phenanthrene, fluoranthene, and pyrene, and for chrysene, benzo[c]phenanthrene, and benz[a]anthracene. Some monohydroxy metabolite isomers of chrysene, benzo[c]phenanthrene, and benz[a]anthracene exhibited low detection frequencies which did not allow for geometric mean calculations. From our study, we established a reference range for the targeted PAHs in the general U.S. population.     

新疆黑山煤液化重质油340-360℃馏分离及分析

用气相色谱/质谱联用仪(GUMS)分析馏程为340-360℃的新疆黑山煤液化重质油,检测出的主要成分为稠环芳烃及其衍生物,此外还有正构烷烃和少量含氧化合物.在超声辅助条件下,对液化重质油进行甲醇萃取,所得第一次甲醇萃取物用硅胶柱层析法分离.各洗脱馏分用GC/MS分析,其可测成分与直接检测相比更丰富,表明合适的预分离对提...     

鞋类塑料中烷基酚检测方法研究

建立了快速检测鞋类塑料中烷基酚（APs）的气相色谱?质谱联用法（GC?MS）。样品采用超声萃取,对萃取溶剂、萃取温度、萃取时间3种条件分别进行了优化。萃取液过滤后用GC-MS检测,外标法定量。结果表明,烷基酚在0.1~10 mg/L浓度范围内呈良好的线性,相关系数（r²）均大于0.995,方法检出限为0.3~1.1 mg/kg,在3个加标水平下的平均回收率为80.7 %~113.3 %,相对标准偏差（RSD,n=6）为1.3 %~8.6 %,该方法简单、快速、准确、稳定可靠,适用于鞋类塑料中APs的检测。     

超高效液相色谱/串联质谱法测定化妆品中15种色素

采用超高效液相色谱-串联电喷雾四极杆质谱在多反应监测模式下测定了特殊功效类化妆品中的15种色素。样品按照不同状态分别进行前处理,目标物以乙酸铵和甲醇为流动相,经C18色谱柱分离。在超高效液相色谱/串联质谱分析过程中以保留时间和离子对（母离子和两个碎片离子）信息比较定性,以母离子和响应值高的碎片离子进行定量。该方法检出限为0.025～1.0μg/g,目标物的添加回收范围为51.3%～107%,相对标准偏差为0.9%～9.8%。