Rapid analysis of polymer homologues and additives with SFE/SFC-MS coupling

A rapid and easy analysis method for polymers is presented. The method involves sample preparation by SFE, separation of the extracted compounds by SFC and simultaneous quantitative detection by FID, as well as identification of unknowns by MS. The applications illustrate how structural research work and routine polymer analysis can be done with this time saving method.     

Supercritical carbon dioxide extraction of lithium-ion battery electrolytes

Two different separator materials (polyethylene fleece – Freudenberg 2190 and porous glass fiber – Whatman^® GF/D) and two different lithium-ion battery electrolytes have been investigated regarding their behavior in an autoclave extraction with supercritical helium head pressure carbon dioxide (sc HHPCO₂). Mixtures of dimethyl carbonate (DMC)/ethylene carbonate (EC) and ethylmethyl carbonate (EMC)/EC, each with 1 mol/L LiPF₆ were used.In addition to these proof of principle experiments, the developed extraction method was further applied to real battery samples. Commercial 18650 cells (after formation and aging) were opened and the jelly roll was extracted with sc HHPCO₂. Extracts were analyzed with gas and ion chromatography (GC, IC). Recovery rates and extract compositions strongly depend on the material of which the electrolyte is extracted. Further structure determination of electrolyte aging products was performed with different ionization modes in GC–mass spectrometry (GC–MS) experiments. Diethyl carbonate (DEC), dimethyl-2,5-dioxahexane dicarboxylate (DMDOHC), ethylmethyl-2,5-dioxahexane dicarboxylate (EMDOHC) and diethyl-2,5-dioxahexane dicarboxylate (DEDOHC) are aging products of electrolyte degradation which were successfully extracted and identified. Their concentrations correlate with solid electrolyte interphase (SEI) growth on the negative electrode which was investigated with scanning electron microscopy (SEM).     

超临界CO2萃取花椒化学成分的研究

本文研究超临界CO2对花椒化学成分的萃取,并通过正交实验确定最佳工艺条件为:萃取时间1.0h,温度45℃,压力33MPa,并探讨了夹带剂对萃取结果的影响。用气相色谱质谱联用(GC-MS)对超临界CO2萃取的花椒化学成分进行了研究。结果表明,超临界CO2萃取法具有提取率高、萃取成分全面、提取时间短、无溶剂残留等优点。     

厚朴抗氧化活性的研究

探讨了压力、温度和时间对厚朴超临界流体萃取工艺的影响,确定了最佳萃取工艺条件是:萃取压力25 MPa、萃取温度40℃、萃取时间3 h.在该工艺条件的基础上加入10%乙醇作夹带剂,不仅大大提高了萃取率,而且大大缩短了萃取时间.用不同极性溶剂索氏抽提与超临界流体萃取相比较,并用OSI法和DPPH自由基清除法对其提取物的抗氧化活性进行了测定.结果发现,OSI法和DPPH自由基清除法实验结果一致,其抗氧化活性的顺序是:BHT＞乙酸乙酯提取物＞氯仿提取物＞超临界CO2萃取物(加入10%乙醇)＞石油醚提取物＞超临界CO2萃取物(未加夹带剂)＞乙醇提取物.厚朴中的抗氧化成分主要是小极性物质,主要存在于石油醚、氯仿和超临界CO2的提取物中.     

Determination of pesticide residues in food matrices using the QuEChERS methodology

The determination of pesticide residues in food matrices is a formidable challenge mainly because of the small quantities of analytes and large amounts of interfering substances which can be co-extracted with analytes and, in most cases, adversely affect the results of an analysis. However, safety concerns require that pesticides of the wide range of chemical properties (including acidic, basic and neutral) should be monitored. Because of the wide variety of food matrices, the sample must initially be cleaned up before final analysis. That is why the analytical chemist is faced with the need to devise new methodologies for determining such residues to be determined in a single analytical run. To accomplish the goal, QuEChERS methodology has been developed. It is a streamlined and effective extraction and cleanup approach for the analysis of diverse analyte residues in food matrices. So far, there have been achieved promising results by liquid or gas chromatography analysis, including pesticides, but also acrylamide, pharmaceuticals and veterinary drugs.     

荆条叶、枝超临界萃取物挥发性化学成分分析

超临界二氧化碳流体法制备北京地区野生芳香植物荆条叶、枝两个部位萃取物。气-质联机分析,计算机质谱库检索结合气相色谱保留指数二维定性,共鉴定出35种挥发性单萜或倍半萜类化合物。主要挥发性成分为β-丁香烯(质量分数:叶44.20%,枝47.15%)、β-甲基紫罗兰酮(质量分数:叶14.17%,枝8.68%)和β-金合欢烯(质量分数叶8.64%,枝10.55%)。     

小决明挥发油的提取及其化学成分的GC-MS分析

分别采用超临界CO2萃取法和水蒸气法提取决明子中的挥发性成分,并用气相色谱、气质联用（GC—MS）测定和分析其化学组分。结果显示：超临界CO2萃取法得到的挥发油的主要成分分别是（Z,Z）-9,12-十八碳二烯酸（26．74％）、油酸（24．15％）、n-十六烷酸（13．99％）、大黄根酚（7．26％）、（E）-9-十八碳烯酸（4．52％）和硬脂酸（4．44％）,挥发油中主要含有脂肪酸（75．88％）和蒽醌（7．26％）,得率高于水蒸气法,其决明挥发油在保持较高的亚油酸和油酸含量同时含有更多其它成分,超临界CO2萃取法比水蒸气法更适于提取决明挥发油。     

农药残留分析中的样品前处理技术研究进展

介绍了近年来出现的超临界流体萃取、加速溶剂萃取、凝胶渗透色谱、固相萃取、固相微萃取、基质固相分散萃取等前处理技术,以及它们在农药残留分析中的应用,并对其发展前景进行了展望。     

原料状况及超临界二氧化碳流体萃取操作条件对当归油萃取率的影响研究

运用超临界流体萃取技术提取当归油 ,综合考察了原料状况 (粒度、水分 )和萃取釜条件 (温度、压力、萃取釜中原料加入量、是否放置填料、填料位置以及SC -CO2 流量 )对当归油萃取率的影响 ,得到较好的超临界流体萃取当归油的条件为 :1L萃取釜装料量 2 5 0 g ,压力 18- 2 0MPa ,温度 4 0℃ ,釜底放置填料 ,时间为 ( 2 - 2 .5 )hr ,原料粒度 ( 4 0 - 6 0 )目 ,含水量 ( 5 .87- 8.7) % ,SC -CO2 流量Q =( 5 - 15 )kg/hr。当归油萃取率可大于 2 .5 7%。