scholarly journals Optimization of Silylation for Parabens Determination by Gas Chromatography-Mass Spectrometry

ALCHEMY ◽  
2016 ◽  
Vol 5 (2) ◽  
pp. 55 ◽  
Author(s):  
Rosalina Djatmika ◽  
Wang-Hsien Ding
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Optimal Condition ◽  
Low Cost ◽  
Gas Chromatography Mass Spectrometry ◽  
Injection Port ◽  
Response Factors ◽  
Chromatography Mass Spectrometry ◽  
Injection Port Temperature ◽  
Off Time

A low cost, environmental friendly and convenient method for parabens derivatization using Gas Chromatography-Mass Spectrometry (GC-MS) analysis is investigated. Derivatization is needed to enhance the thermal stability, detectability, and volatility of parabens to make them amenable for gas chromatographic analysis. This method involved on-line derivatization by silylating reagent: N-Methyl-N-tert-butyldimethylsilyltrifluoroacetamide (MTBSTFA), N,O-bis (trimethylsilyl) trifluoroacetamide (BSTFA), N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA), and N,O-bis(trimethylsilyl)acetamide (BSA). The variables affected the derivatization process, such as, types and volumes of silylating reagents, injection port temperature, and purge-off time, were evaluated to obtain the optimal condition for determination of parabens. The Relative Response Factors (RRF) was used as a parameter of parabens derivatization efficiency to obtain the best compromise condition of each variable. On a comprehensive level, a comparison of the optimal condition of each silylating reagent was evaluated. Moreover, 1 µL of MSTFA  at 260°C of injection port temperature and 2.5 min purge-off time (in splitless mode) obtained the most effective of derivatization process.

scholarly journals Development of a Method for Rapid Determination of Morpholine in Juices and Drugs by Gas Chromatography-Mass Spectrometry

2018 ◽  
Vol 2018 ◽  
pp. 1-8 ◽  
Author(s):  
Mengsi Cao ◽  
Pingping Zhang ◽  
Yanru Feng ◽  
Huayin Zhang ◽  
Huaijiao Zhu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Sodium Nitrite ◽  
Recovery Rate ◽  
Rapid Determination ◽  
Low Cost ◽  
Extraction Process ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard

A reliable derivatization method has been developed to detect and quantify morpholine in apple juices and ibuprofen with gas chromatography-mass spectrometry. Morpholine can react with sodium nitrite under acidic condition to produce stable and volatile N-nitrosomorpholine derivative. In this experiment, various factors affecting the derivatization and extraction process were optimized, including volume and concentration of hydrochloric acid, quantity of sodium nitrite, derivatization temperature, derivatization time, extraction reagents, and extraction time. The derivative was extracted with dichloromethane and determined by gas chromatography-mass spectrometry. The linearity range of morpholine was 10–500 μg·L−1 with good correlation, and limits of detection (LOD) and limits of quantification (LOQ) were 7.3 μg·L−1 and 24.4 μg·L−1, respectively. Low, medium, and high concentrations of morpholine were added in apple juices and ibuprofen samples to evaluate standard recovery rate and relative standard deviation. The spiked recovery rate ranged from 94.3% to 109.0%, and the intraday repeatability and interday reproducibility were 2.0%–4.4% and 3.3%–7.0%, respectively. The developed method has good accuracy and precision. This quantitative method for morpholine is simple, sensitive, rapid, and low cost and can successfully be applied to analyze the residual morpholine in apple juices and drug samples.

Gas chromatography–mass spectrometry analyses of encapsulated stable perovskite solar cells

Science ◽  
2020 ◽  
Vol 368 (6497) ◽  
pp. eaba2412 ◽  
Author(s):  
Lei Shi ◽  
Martin P. Bucknall ◽  
Trevor L. Young ◽  
Meng Zhang ◽  
Long Hu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solar Cells ◽  
Low Cost ◽  
Perovskite Solar Cells ◽  
Gas Chromatography Mass Spectrometry ◽  
International Electrotechnical Commission ◽  
Chromatography Mass Spectrometry ◽  
Freeze Test ◽  
Conversion Efficiencies

Although perovskite solar cells have produced remarkable energy conversion efficiencies, they cannot become commercially viable without improvements in durability. We used gas chromatography–mass spectrometry (GC-MS) to reveal signature volatile products of the decomposition of organic hybrid perovskites under thermal stress. In addition, we were able to use GC-MS to confirm that a low-cost polymer/glass stack encapsulation is effective in suppressing such outgassing. Using such an encapsulation scheme, we produced multi-cation, multi-halide perovskite solar cells containing methylammonium that exceed the requirements of the International Electrotechnical Commission 61215:2016 standard by surviving more than 1800 hours of the Damp Heat test and 75 cycles of the Humidity Freeze test.

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