GC-MS-Analysis =============== 1. 调用数据; 2. Mass Spectrometry and 谱图检索报告 (选择屏幕); 3. Alt+S+S用于背景删除 4. 生成百分比报告. 5. 修改runlib(用记事本打开)相关的检索名与峰面积; 6. 再次生成百分比报告, 并返回记事本, 填写保留时间后面的百分比. .. raw:: html :file: GC-MS-Analysis-1.html .. raw:: html :file: GC-MS-Analysis-2.html .. raw:: html :file: GC-MS-Analysis-3.html .. raw:: html :file: GC-MS-Analysis-5.html 进样选择方法: 25-1适用于浓度低的样品进样; 100-1适用于浓度高的进样; 还有6-1. 同分异构体虽然质谱图一样，但是保留时间必然有区别。 销售分析调香OEB销售闭合回路 ------------------------- 销售=>分析=>调香=>OEB=>销售 闭合回路 GCMS 原料分析 --------------- 要单独用表格记录原料分析， 将待测原料用酒精进行稀释5%，然后使用602280方法(浓度较高)，取0.5ml进行进样，注意用PC编号和中文名字进行命名进样。 `FA13008 The First Experiment `_ ------------------------------ The first experiment of SDE was done and analysed by Tongjia. You can download the source code by clicking this link :download:`The First Experiment ` `FA13008 TIC `_ ---------------- You can download the source code by clicking this link :download:`FA13008 TIC ` `FA13008 Pentane vs t-butyl methyl mester `_ -------------------------- You can download the source code by clicking this link :download:`FA13008 Pentane vs t-butyl methyl mester` `FA13008 t-butyl methyl mester `_ ------------------------- You can download the source code by clicking this link :download:`FA13008 t-butyl methyl mester` `FA13008 Pure vs SDE `_ ------------------------------- You can download the source code by clicking this link :download:`FA13008 Pure vs SDE ` `The impact of vapor pressure and mole fraction on the recovery of different components using SDE `_ -------------------------------------------------- You can download the source code by clicking this link :download:`The impact of vapor pressure and mole fraction ` `TheimpactofvaporpressureandmolefractionandlogP `_ ---------------------------------------------- 由正戊烷萃取出来的FA13008样品，头香保留比较好；而由二氯甲烷萃取出来的FA13008整体性保留比较好，尤其是中段及后段的香味。 `The Four important factors on SDE Efficiency `_ ------------------------------------ You can download the source code from here :download:`source code `. `FA13008 CH2Cl2 `_ ----------------------------- You can download the source code from here :download:`source code `. `FA13008_Comparison_of_Solvent.html `_ ----------------------------- FA13008_Comparison_of_Solvent GC-LC Concordance Software -------------------------- GC-LC concordance software dramatically enhances the possibilities of chromatography on complex products and chromatographic fingerpringts by solving retention time shifting in complex chromatograms comparison. Optimization of Working Parameters ------------------------------------ The best compromise between the above-mentioned parameters(:strong:`Solvent`, :strong:`Salting-out`, :strong:`Distillation-Extraction Time`, :strong:`Oxygen Effect`) can be determined empirically. :strong:`Method 1`: `Optimization acheived by varying four variables: 1. temperature of the sample; 2. temperature of the solvent baths; 3. the coolant temperature; 4. the isolation time `_ :strong:`Method 2`: `A face centred cube experimental design `_ :strong:`Conclusions`: - Recoveries differ, depending on the volatilities and solubilities of the analytes in the solvent. - Too high a solvent temperature leads to decreasing extraction efficiencies. - The isolation time decreases as the sample temperature increases. :strong:`Method 3`: Another alternative to optimize SDE working conditions lies in the use of a mathematical model. SDE工作条件影响汇总 -------------------- - 溶剂的影响:: 许多比水的密度高或者低的溶剂用于SDE实验, 并做了相应的比较: 二氯甲烷, 正戊烷, 异戊烷, 正己烷, 氯仿, 乙酸乙酯, 乙醚, 叔丁基甲醚, 三氯氟甲烷, 1,1,2-三氯三氟乙烷以及溶剂混合物比如正戊烷/乙醚. 通常得出来的结论是, 二氯甲烷一般来说是萃取的最好溶剂. 对于特定的化合物来说, 其他的溶剂可能表现出更高的效率, 但是实用性最广的仍然是二氯甲烷, 如图5展示出来的半挥发性化合物. `Comparison of solvent efficiency. Average recoveries are 47%, 59%, 53%, 58% and 36% `_ - 盐析效应:: 为降低挥发组分在水中的溶解度, 向样品烧瓶中加入盐溶液被提出来了. 这看起来只是特别适合提取极性物质的回收率, 例如香豆素或者2-苯乙醇; 但是, 香兰素和乙基香兰素提取量仍然可以忽略. - 蒸馏-萃取时间:: 最优化的蒸馏-萃取时间从实验上已经被求证过: 达到48h的蒸馏萃取时间已经被验证可以从肥皂中提取挥发度比较 低的化合物(比如: 肉桂醇, 2-苯乙醇). 值得注意的是, 含有油脂类的基质会急剧增加获取可接受的回收率的时间 `Lipid Matrix `_