Atmospheric Pressure Chemical Ionization
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Molecules ◽  
2021 ◽  
Vol 26 (22) ◽  
pp. 6760
Author(s):  
De-Yi Huang ◽  
Meng-Jiy Wang ◽  
Jih-Jen Wu ◽  
Yu-Chie Chen

Atmospheric pressure chemical ionization (APCI)-mass spectrometry (MS) and electrospray ionization (ESI)-MS can cover the analysis of analytes from low to high polarities. Thus, an ion source that possesses these two ionization functions is useful. Atmospheric surface-assisted ionization (ASAI), which can be used to ionize polar and nonpolar analytes in vapor, liquid, and solid forms, was demonstrated in this study. The ionization of analytes through APCI or ESI was induced from the surface of a metal substrate such as a titanium slab. ASAI is a contactless approach operated at atmospheric pressure. No electric contacts nor any voltages were required to be applied on the metal substrate during ionization. When placing samples with high vapor pressure in condensed phase underneath a titanium slab close to the inlet of the mass spectrometer, analytes can be readily ionized and detected by the mass spectrometer. Furthermore, a sample droplet (~2 μL) containing high-polarity analytes, including polar organics and biomolecules, was ionized using the titanium slab. One titanium slab is sufficient to induce the ionization of analytes occurring in front of a mass spectrometer applied with a high voltage. Moreover, this ionization method can be used to detect high volatile or polar analytes through APCI-like or ESI-like processes, respectively.


2021 ◽  
Vol 10 (5) ◽  
pp. 3534-3537
Author(s):  
Narayan Shrivas

As a result of the devotion of The Limit of N-Nitrosodimethylamine (NDMA), a rapid and selective LC/MS/MS technique was created and validated for Empagliflozin, Linagliptin, and Metformin Hydrochloride Extended-Release Tablets. The ionization mode of Atmospheric pressure chemical ionization (APCI) was used with high-performance liquid chromatography-tandem mass spectrophotometry (LC-MS/MS). Separation of N-Nitrosodimethylamine (NDMA) was performed on Inertsil ODS-4 (250 mm X 4.6 mm), 5μm column with a run time of 40 minutes. A mixture of Methanol and Buffer solution (630 mg of ammonium format into 1000 mL of purified water) in the ratio of (10:90, v/v) was used as the mobile phase A. A mixture of acetonitrile and methanol comprised the mobile phase B in the ratio of (50:50) % v/v. Analytes were extracted from Empagliflozin, Linagliptin, and Metformin Hydrochloride Extended-Release Tablets. According to the International council for Harmonization of technical requirement for Pharmaceuticals for Human Uses (ICH) standards, the accuracy, precision, selectivity, recovery, and stability of the method have been validated. Over a concentration range of 0.4 -3.6 ng/mL, the technique exhibited linearity. for N- Nitrosodimethylamine of Empagliflozin, Linagliptin, and Metformin Hydrochloride Extended-Release Tablets with an acceptable correlation coefficient applies (1/X2) linear regression with weights A pharmaceutical study can benefit from this method because it is simple, fast, precise, and accurate, making it ideal for pharmaceutical research.


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.


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