开发和验证一种改进的、基于薄膜固相微萃取的标准气体产生瓶,用于可重复生成气体标准。

ty10086 提交于 周三, 08/25/2021 - 16:52
文章英文标题
Development and validation of an improved, thin film solid phase microextraction based, standard gas generating vial for the repeatable generation of gaseous standards.
正文
本文介绍了一种新型薄膜固相微萃取( TF-SPME )标准气体发生瓶的研制和验证,该标准气体发生瓶适用于GC-MS分析和质量控制的可重复生成气体标准。采用纯聚二甲基硅氧烷( PDMS )、二乙烯烯基苯( DVB / PDMS )、亲水亲油平衡( HLB / PDMS )和Carboxen ( Car / PDMS )吸附剂的碳网膜,然后添加改性McReynolds标准的苯、2 -戊酮、1 -硝基丙烷、吡啶、1 -戊醇、辛烷、十二烷和十六烷。吸附强度按上述顺序确定,纯PDMS吸附能力最弱,Car / PDMS吸附能力最强。虽然较弱的、纯的PDMS气体产生瓶将McReynolds探针的仪器超载量转移到用于萃取的1.1  毫米DVB / PDMS固相微萃取箭头上,但以Car / PDMS TF-SPME为吸附剂制备的瓶未能提供比1 -硝基丙烷挥发量更低的分析物的持续检测量。研究发现,基于DVB / PDMS和HLB / PDMS的小瓶保持了对被测分析物的最佳吸附能力,提供了足够强的吸附强度,在10次重复中不会出现任何损耗,同时仍然提供了一贯量的常规McReynolds组分。而且,所有被测分析物的活体% RSD均小于5 %,这些HLB和DVB瓶具有很好的重复性。有目的地将瓶子提交200个加速耗尽萃取物( 1.1   mm DVB / PDMS箭头55℃3   min ),DVB / PDMS制备的瓶子耗尽量分别为33 %、38 %、34 %、33 %、40 %、33 %,HLB / PDMS制备的瓶子耗尽量分别为21 %、16 %、12 %、31 %、16 %、0 %,苯、2 -戊酮、1 -硝基丙烷、吡啶、1 -戊醇、辛烷。采用用户典型的萃取条件( 50 / 30  μm DVB / Car / PDMS SPME光纤,35℃,1   min ),经300次萃取/解吸循环后,HLB / PDMS基瓶体无损耗,相对标准偏差为1.1 % ~ 3.0 %。最后,为了验证其真实世界适用性,采用DVB / PDMS小瓶对市售DVB / PDMS SPME箭头的纤维间重复性进行了评估,结果显示单个包的箭头在统计上相似( 95 %置信度下的ANOVA )。
文章内容(英文)
This work presents the development and validation of novel thin film solid phase micro extraction (TF-SPME) based standard gas generating vials suitable for repeatable generation of gaseous standards for GC-MS analysis and quality control. The vials were developed using carbon mesh membranes loaded with pure polydimethylsiloxane (PDMS), divinylbenzene (DVB/PDMS), hydrophilic-lipophilic balance (HLB/PDMS), and carboxen (Car/PDMS) sorbents that were then spiked with modified McReynolds standards including benzene, 2-pentanone, 1-nitropropane, pyridine, 1-pentanol, octane, dodecane, and hexadecane. Sorbent strength was determined to follow the aforementioned order, with pure PDMS presenting the weakest sorption capabilities and Car/PDMS the strongest. While the weaker, pure PDMS based gas generating vials transferred an instrument-overloading amount of McReynolds probes to the 1.1 mm DVB/PDMS SPME arrows used for extraction, vials prepared using Car/PDMS TF-SPME as a sorbent failed to provide consistently detectable amounts of analytes less volatile than 1-nitropropane. The DVB/PDMS and HLB/PDMS based vials were found to maintain optimal sorption capabilities for the tested analytes, providing a sorption strength strong enough to not exhibit any depletion in 10 replicate runs, while still delivering a consistent amount of all the regular McReynolds components. Moreover, with intra-vial%RSDs of 5% or less for all analytes tested, these HLB and DVB vials were found to deliver very good repeatability. After purposely submitting vials to 200 accelerated depletion extractions (1.1 mm DVB/PDMS arrow at 55 °C for 3 min), vials prepared with DVB/PDMS were found to deplete by 33%, 38%, 34%, 33%, 40%, and 33% while vials prepared with HLB/PDMS were found to deplete by 21%, 16%, 12%, 31%, 16% and 0% for benzene, 2-pentanone, 1-nitropropane, pyridine, 1-pentanol, and octane, respectively. When user typical extractions conditions were used instead (50/30 μm DVB/Car/PDMS SPME fiber at 35 °C for 1 min), no depletion could be observed from the HLB/PDMS based vial while%RSDs ranged from 1.1-3.0% after the 300 extraction/desorption cycles. Finally, in efforts to demonstrate its real world applicability, the DVB/PDMS vial was used to evaluate the inter-fiber repeatability of commercial DVB/PDMS SPME arrows, with results demonstrating that arrows from a single package were statistically similar (ANOVA at 95% confidence).
来源出处
Journal|[J]Journal of Chromatography AVolume 1632, 2020. PP 461541-461541
DOI
https://doi.org/10.1016/j.chroma.2020.461541

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备注说明:

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