仪器方法： Injector: Split/splitless, 1 min, 320℃ , 1.5 μL injection volume with Merlin seal Carrier gas: He, 0.6 mL/min, const. flow Column: TRACE ? -50MS, 10 m x 0.1 mm x 0.1 μm Oven Temp. Program: 140 ℃ , 1 min 10 ℃ /min to 240℃ 5 ℃ /min to 270℃ 30 ℃ /min to 280℃ 4 ℃ /min to 290℃ 30 ℃ /min to 315℃ 3 ℃ /min to 330℃ Transfer line 300℃ ion source 280℃ Ionization: EI, 45 eV pos. Scan Mode: Multiple ion detection mode (MID) Resolution: 8,000, 10% valley definition Cycle Time: 0.8 s/scan
参考文献 [Application Note: 30126] Fast GC/HRMS Quantification of 16 EC Priority PAH ComponentsKarl Speer, Technical University Dresden, Institute of Food Chemistry, Dresden, Germany, Katja Ziegenhals, Wolfgang Jira, Federal Research Centre for Nutrition and Food (BfEL), Kulmbach, Germany, Hans-Joachim Huebschmann, Thermo Fisher Scientific, Bremen, Germany Contents of polycyclic aromatic hydrocarbons (PAH) and phenolic substances in Frankfurter-type sausages depending on smoking conditions using glow smoke Margarete P?hlmann , Alexander Hitzel , Fredi Schw?gele , Karl Speer , Wolfgang Jira Polycyclic aromatic hydrocarbons (PAH) and phenolic substances in meat products smoked with different types of wood and smoking spices Alexander Hitzel , Margarete P?hlmann , Fredi Schw?gele , Karl Speer , Wolfgang Jira
应用案例四：短链氯化石蜡
SCCP C 10 H 17 Cl 5 –“CP3”标准物质色谱图
Sample Preparation
样品准备和标准物质由 Environment Canada, Burlington ON, Canada 提供。 1. 标准物质 SCCP C 10 H 17 Cl 5 – “CP3” 2. 混合物 SCCPs C10-13 55.5% Cl 环己烷 3. 包含 C13 内标的基质提取样品
Gas Chromatography
GC Column：Trace Gold TR-5MS 30m x 0.25mm, 0.1 μm film GC Liner：Single taper splitless Injector temp： 220 ℃ Splitless time：3 minutes Transfer line：220℃ Column Flow：1 mLmin -1 , constant flow
Mass Spectrometry
Electron capture negative chemical ionisation was used to analyse SCCPs. EC NCI Buffer Gas：Isobutane and ammonia Source Pressure：6x10-4 mBar Electron engery：90 eV Emission current：0.3 mA Ion source temp：80-95 ℃ Scan Multiple Ion Detection (MID)
参考文献 Analysis of Short Chain Chlorinated Paraffins (SCCPs) using High Resolution Mass Spectrometry and Negative Chemical Ionization (NCI GC-HRMS) Frank Theobald1, Heinz Mehlmann2, Dirk Krumwiede2 & Kyle D’Silva2 1. Environmental Consulting, Cologne, Germany 2. POPs Center of Excellence, Thermo Fisher Scientific,Bremen, Germany
应用案例五：荷尔蒙 类固醇及农药
● EPA Method 1698: Steroids and Hormones in Water, Soil, Sediment,and Biosolids by HRGC/HRMS 高分辨气相色谱与高分辨磁质谱联用分析水体、土壤、沉积物及生物体中的类固醇和荷尔蒙 ● EPA Method 1699: Pesticides in Water,Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS 高分辨气相色谱与高分辨磁质谱联用分析水体、土壤、沉积物及生物体中的农药
参考文献 ● EPA Method 1698: Steroids and Hormones in Water, Soil, Sediment,and Biosolids by HRGC/HRMS ● EPA Method 1699: Pesticides in Water,Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS
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【生活中的仪器检测】有奖征文
LC-MS实验瓶颈的突破与优化
