Identificación de Creatinina y Diciandiamida en suplementos deportivos de Monohidrato de Creatina en polvo por UHPLC/MS-MS
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Date
2022
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Universidad Nacional de Trujillo
Abstract
La creatinina y diciandiamida son impurezas orgánicas derivadas de un mal proceso de manufactura, ya sea una errónea síntesis química o escasos lavados con solventes especiales. El presente estudio tuvo como finalidad identificar creatinina y diciandiamida en suplementos de monohidrato de creatina en polvo por UHPLC/MS-MS. Para la separación cromatográfica se utilizó como fase móvil, una solución A compuesta por ácido fórmico al 0,1% y una Solución B compuesta por Acetonitrilo y Solución A. Usando una columna de fase reversa (C18) Acquity UHPLC HSS TT3 (150 x 2,1 mm) y relleno de 1,8 µm, acoplado a un analizador de masas triple cuádrupolo y electropulverización positiva. Identificando relaciones masa carga (m/z) de 114 y 86 para la creatinina presentes en las muestras MP, RC y KL. A su vez se encontró picos base de 85 m/z confirmando la presencia de diciandiamida solo en las muestras RC y KL
ABSTRACT Creatinine and dicyandiamide are organic impurities derived from a bad manufacturing process, whether it is an erroneous chemical synthesis or few washings with special solvents. The purpose of this research work was to identify creatinine and dicyandiamide in powdered creatine monohydrate supplements by UHPLC/MS-MS. For the chromatographic separation, a solution A composed of 0.1% formic acid and a Solution B composed of Acetonitrile and Solution A were used as mobile phase. Using a reverse phase column (C18) Acquity UHPLC HSS TT3 (150 x 2 .1 mm) and 1.8 µm filler, coupled to a triple quadrupole mass analyzer and positive electrospray. Identifying mass- charge ratios (m/z) of 114 and 86 for creatinine present in samples MP, RC and KL. In turn, base peaks of 85 m/z were found, confirming the presence of dicyandiamide only in the RC and KL samples.
ABSTRACT Creatinine and dicyandiamide are organic impurities derived from a bad manufacturing process, whether it is an erroneous chemical synthesis or few washings with special solvents. The purpose of this research work was to identify creatinine and dicyandiamide in powdered creatine monohydrate supplements by UHPLC/MS-MS. For the chromatographic separation, a solution A composed of 0.1% formic acid and a Solution B composed of Acetonitrile and Solution A were used as mobile phase. Using a reverse phase column (C18) Acquity UHPLC HSS TT3 (150 x 2 .1 mm) and 1.8 µm filler, coupled to a triple quadrupole mass analyzer and positive electrospray. Identifying mass- charge ratios (m/z) of 114 and 86 for creatinine present in samples MP, RC and KL. In turn, base peaks of 85 m/z were found, confirming the presence of dicyandiamide only in the RC and KL samples.
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Keywords
Suplementos deportivos. Impurezas. Creatina