scholarly journals Eco-Friendly Direct GC–MS Method for Estimation of Niacin and Related Impurities Involving Pyridine in Food Supplements

Separations ◽  
2021 ◽  
Vol 8 (4) ◽  
pp. 46
Author(s):  
Atiah H. Almalki ◽  
Ibrahim A. Naguib ◽  
Fatma F. Abdallah

Niacin is a water-soluble vitamin whose deficiency causes many disorders and diseases, including pellagra and high blood cholesterol. Herein, niacin and four common impurities, isonicotinic acid (ISO), 5-ethyl-2-methylpyridine (MP), pyridine-2, 5-dicarboxylic acid (PDC) and pyridine PYR, are simultaneously analyzed, where PYR is known as potentially nephrotoxic and hepatotoxic. The separation of a mixture using gas chromatography–mass spectroscopy (GC–MS) without any derivatization steps was the main target. Many studies have been published to study Niacin and its impurities using colorimetry and HPLC. GC–MS was selected to study the analyzed mixture owing to its known sensitivity and selectivity. In this study, a single quadrupole mass spectrometer operated in selected ion monitoring (SIM) mode at an electron ionization energy of 70 eV was applied for the quantitative analysis of Niacin. Helium was used as the carrier gas and adjusted to run through an HP-5ms (5%-phenyl)-methylpolysiloxane column. Statistical analysis proved that this method is equally effective as the previously reported method. Importantly, this study was eco-friendly as compared to the reported high performance thin layer chromatographic method (HPTLC). Finally, this study provides a new and valid eco-friendly method analysis to determine the concentration of niacin and its common impurities at very low concentration. Conclusion: A simple, rapid accurate and green GC–MS analytical method was developed and validated to determine niacin and its related official impurities.

2019 ◽  
Vol 35 (4) ◽  
pp. 1344-1351
Author(s):  
N. H. M. Rubel Mozumder ◽  
Most. Jesmin Akhter ◽  
Anwara Akter Khatun ◽  
Mohammad Rokibuzzaman ◽  
M. Akhtaruzzaman

A high performance liquid chromatographic method (HPLC) equipped with photodiode array detector (PDA) has been used to determine the water-soluble vitamin B complex ( B1, B2, B3, and B6) in eleven selected vegetables of Bangladesh. The results showed varied levels of vitamin B-complexes. Precisely, Thankuni leaves showed the highest contents of vitamin B1; 0.19 mg/100 g, and vitamin B2; 0.25 mg/100g. Higher content of vitamin B3 (0.59 mg/100 g) were quantified in Coriander leaves, but absent in Jute leaves. On the other hand, the maximum quantified amount of B6 (0.73 mg/100 g) was detected in Carrot. In contrast, there was no detectable vitamin B6 in Jute, and Mint leaves and Cabbage. The findings of the current study may supplement the current Food Composition Table for Bangladesh (FCTB) by providing nutritional information of vitamin B complex in leafy and non-leafy vegetables which can also be used for calculating the habitual dietary intake and/or nutritional survey purposes.


2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Atiah H. Almalki ◽  
Essraa A. Hussein ◽  
Ibrahim A. Naguib ◽  
Eglal A. Abdelaleem ◽  
Hala E. Zaazaa ◽  
...  

Novel, accurate, selective, and rapid high-performance liquid chromatography mass spectrometry method was developed for simultaneous analysis of amoxicillin trihydrate, dicloxacillin sodium, and their official impurity 6-aminopenicillanic acid. The chromatographic separation was carried out by applying the mixture on a C18 column (3.5 µm ps, 100 mm × 4.6 mm id) using acetonitrile:water (65 : 35 by volume) as a mobile phase within only 4 min. The quantitative analysis was executed using single quadrupole mass spectrometer in which electrospray ionization, selected ion monitoring, and negative mode were operated. The retention times were 1.61, 2.54, and 3.50 mins for amoxicillin, 6-aminopenicillanic acid, and dicloxacillin, respectively. The method was validated in linear ranges of 2–28 µg mL−1, 2–35 µg mL−1, and 1–10 µg mL−1 for amoxicillin, dicloxacillin, and 6-aminopenicillanic acid, respectively. The results obtained from the suggested HPLC/MS were statistically compared with those obtained from the reported HPLC method, where no significant difference appeared respecting accuracy and precision. According to the analytical eco-scale assessment method, the proposed method was proved to be greener than the reported one, where the analysis time and the amount of the wasted effluent decreased.


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