Solvent-free headspace GC/MS method for sensitive screening of N-nitrosodimethylamine in drug products

2021 ◽  
Author(s):  
Do Hee Lee ◽  
Seongchul Park ◽  
Su Hyeon Hwang ◽  
Jeongmi Lee ◽  
Han Bin Oh ◽  
...  

A solvent-free headspace gas chromatography – mass spectrometry (SF-HS-GC/MS) method was developed and validated for screening of N-nitrosodimethylamine (NDMA) in various active pharmaceutical ingredients (APIs) and drug products. Experimental parameters...

2021 ◽  
Vol 3 (3) ◽  
Author(s):  
Yinzheng Ma ◽  
Yingying Wen ◽  
Jinping Chen ◽  
Yunxia Zhang ◽  
Haiying Zhang ◽  
...  

AbstractA rapid and sensitive headspace gas chromatography-mass spectrometry (HS-GC–MS) method was established for the determination of benzyl isothiocyanate (BITC) in the peel, pulp, and seeds of Carica papaya Linn. Tween 80 solution with a concentration of 0.002% (w/v) was chosen as a headspace medium for solving the poor solubility of BITC in water without using organic solvents and ensuring high headspace efficiencies. Extraction parameters had been evaluated and optimized by using an orthogonal design with an OA9(34) table. Optimal headspace conditions were obtained when vials were equilibrated at 80 °C for 20 min at a stirring speed of 375 rpm. The calibration curve obtained by using GC–MS was linear in a concentration range of 10–320 ng/mL. The recoveries of peel, pulp, and seeds ranged from 97.3 to 100.6% with RSDs less than 3.0%. The method is simple, rapid, sensitive, and environmentally friendly. It is suitable for analyzing BITC in papaya fruit and is expected to have important application potential in the extraction of water-insoluble volatile components in foods, plants, medicines, and other samples.


Foods ◽  
2019 ◽  
Vol 8 (6) ◽  
pp. 205
Author(s):  
Wei Zhang ◽  
Xianrui Liang

In this study, natural deep eutectic solvents (NADESs) were used as both the extraction and dilution matrix in static headspace gas chromatography-mass spectrometry (SHS-GC-MS) for the analysis of volatile components in Ipomoea cairica (L). Sweet (ICS) leaves. Six NADESs were prepared and the NADESs composed of choline chloride and glucose with a 1:1 molar ratio containing 15% water were preferred due to the better peak responses. A total of 77 volatiles in ICS leaves were detected and tentatively identified by mass spectral matching with the US National Institute of Standards and Technology (NIST, 2014) Mass Spectral Library and the retention index-assisted qualitative method. These 77 volatile components were mainly terpenoids, aromatics, and aliphatics. Among them, β-elemene, β-caryophyllene, α-humulene, and 2, 4-di-tert-butylphenol were found to be the main components. This investigation verified that the use of NADESs is an efficient green extraction and dilution matrix of the SHS-GC-MS method for direct volatile component analysis of plant materials without extra extraction work.


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