scholarly journals Development of an Atmospheric Pressure Chemical Ionization Interface for GC-MS

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3253
Author(s):  
Christian Lipok ◽  
Florian Uteschil ◽  
Oliver J. Schmitz

A closed atmospheric pressure chemical ionization (APCI) ion source as interface between a gas chromatograph (GC) and a triple quadrupole mass spectrometer (QqQ-MS) was developed. The influence of different ion source conditions, such as humidity, make-up gas flow, and the position of the GC column, were investigated and determined as main factors to increase sensitivity and repeatability of the system. For a performance test under real conditions, the new APCI ion source was used for the determination of plant protection products in commercially available coffee beans from Vietnam. The ionization behavior was investigated and the majority of the analytes were detected as [MH]+, [M]+∙, or as characteristic fragment ions, which have been assigned to ion source fragmentation. The developed GC-MS methods are based on tandem MS (MS/MS) and revealed for the plant protection products limits of detection (LOD) between 1 and 250 pg on column and relative standard derivations for all compounds < 16%. The used ultrasonic solid–liquid extraction yielded recovery rates of approximately 60 to 100%. Residues of herbicide methyl esters, organophosphorus compounds, and organonitrogen compounds have been detected in the analyzed coffee beans.

Author(s):  
N. Devanna ◽  
Indhu Priya Mabbu ◽  
G. Sumathi

The main objective of the present research study is to develop and validate a sensitive, specific, accurate and precise LC-MS method for the determination of p-Chloroaniline and (S)-5-Chloro-α-(cyclopropylethynyl)-2- amino-α- (trifluoromethyl) benzene methanol in Efavirenz bulk form. The effective separation of p-Chloroaniline and (S)-5-Chloro-α-(cyclopropylethynyl)-2- amino-α- (trifluoromethyl) benzene methanol were achieved by using Hypersil BDS (C18, 100 x 4.6 mm, 3 µm) column and a solvent system of Buffer (0.1% Formic acid in water): Methanol (30:70 v/v) with a flow rate of 0.4 ml/min. The p-Chloroaniline and (S)-5-Chloro-α-(cyclopropylethynyl)-2- amino-α-(trifluoromethyl) benzene methanol were monitored on mass spectrometer coupled with atmospheric pressure chemical ionization, positive polarity mode and quadrapole mass analyzer. The Retention time of p-Chloroaniline, (S)-5-Chloro-α-(cyclopropylethynyl)-2- amino-α- (trifluoromethyl) benzene methanol and Efavirenz were found at 5.7min, 7.6min and 11.1min resepectively. The detection limit and quantification limit were observed at 0.25ppm and 0.75 ppm respectively for both p-Chloroaniline and (S)-5-Chloro-α-(cyclopropylethynyl)-2- amino-α-(trifluoromethyl) benzene methanol. Those analytes were linear in the concentration ranges from 0.75ppm to 3.75ppm and the percentage relative standard deviation of six replicates of same concentrations of both the analytes were less than 10%. Hence this method was effective in separation and determination of p-Chloroaniline and (S)-5-Chloro-α-(cyclopropylethynyl)-2- amino-α- (trifluoromethyl) benzene methanol in Efavirenz.


2015 ◽  
Vol 50 (4) ◽  
pp. ii-ii
Author(s):  
Dilshadbek Tursunbaevich Usmanov ◽  
Lee Chuin Chen ◽  
Zhan Yu ◽  
Shinichi Yamabe ◽  
Shigeyoshi Sakaki ◽  
...  

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