Identification of l‐carnitine and its impurities in food supplement formulations by online column‐switching liquid chromatography coupled with linear ion trap mass spectrometry. Issue 2 (19th December 2016)

• Record Type: Journal Article
• Authors: Wang, Hang; Xie, Sijun
• Is Part Of: Journal of separation science. Volume 40:Issue 2(2017)
• Page Start: 431
• Page End: 441
• Publication Date: 2016-12-19
• Subjects: l‐carnitine -- Column‐switching -- High‐performance liquid chromatography -- Impurities -- Mass spectrometry; Separation (Technology) -- Periodicals; Chromatographic analysis -- Periodicals; 543.089
• DOI: 10.1002/jssc.201600652
• Languages: English
• ISSNs: 1615-9306

Abstract

Abstract : The identification of impurities inl‐ carnitine by mass spectrometry is difficult because derivative reagents or ion pair reagents are usually used to separate and increase the retention ofl‐ carnitine on the reversed‐phase column. In this study, four impurities including 3‐chloro‐2‐hydroxy ‐N, N, N ‐trimethylpropan‐1‐aminium, 3‐cyano‐2‐hydroxy ‐N, N, N ‐trimethylpropan‐1‐aminium, 3‐carboxy‐ N, N, N ‐trimethylprop‐2‐en‐1‐aminium, and 4‐chloro‐2, 3, 4‐trihydroxy‐ N, N, N ‐trimethylbutan‐1‐aminium were identified inl‐ carnitine and its tablets by using two‐dimensional column‐switching high‐performance liquid chromatography coupled with linear ion trap mass spectrometry. The first column was a C8 column at a flow rate of 0.15 mL/min; the detection wavelength was 220 nm. The second column was an Acclaim Q1 column using a gradient elution program with aqueous 30 mM ammonium acetate (pH 5.0) and acetonitrile as the mobile phase at a flow rate of 0.5 mL/min. The mass fragmentation patterns and structural assignments of impurities were studied, and the quantitative validation of three impurities was further investigated. The linearity ( r 2 ) was found to be >0.99, with ranges from 0.2 to 50 ng/mL and 0.1 to 10 ng/mL. The method was used successfully for determination of impurities in five samples ofl‐ carnitine and tablets.