Dal Molin Thaís Ramos, da Silveira Géssica Domingos, Leal Gabriela Camera, Müller Larissa Sabo, Muratt Diana Tomazi, de Carvalho Leandro Machado, Viana Carine
Graduate Programme in Pharmaceutical Sciences, Federal University of Santa Maria, Santa Maria, RS, Brazil.
Chemistry Institute State University of Campinas, Campinas, SP, Brazil.
Biomed Chromatogr. 2019 Nov;33(11):e4669. doi: 10.1002/bmc.4669. Epub 2019 Aug 30.
The extent of adulteration of dietary supplements has significantly increased in recent years. This situation worries health authorities and requires auxiliary analytical tools for the investigation of illegal substances purposely added. Ion exchange chromatography with conductivity detection is a consolidated analytical technique for the determination of inorganic compounds in various matrices. This technique has been applied to the pharmaceutical characterization of mainly impurities and degradation products. This work presents a new approach to ion exchange chromatography as a screening method to investigate the presence of amfepramone, femproporex, sibutramine, bisacodyl and amiloride in dietary supplements advertised for weight loss. The method was optimized and validated using a Metrosep C4 100/4.0 cation exchange column. The mobile phase consisted of 1.8 mm HNO containing 2% acetonitrile (v/v), with a flow rate of 0.9 ml min , and nonsuppressed conductivity detection was applied. The limits of detection and quantification varied from 1.01 to 3.62 mg L and from 1.48 to 8.72 mg L , respectively. The proposed method was successful applied to 78 solid dietary supplement samples, in two of which adulterations were found. Moreover, ion exchange chromatography with conductivity detection could be easily used for quality control without prior complex sample pre-treatment.
近年来,膳食补充剂的掺假程度显著增加。这种情况令卫生当局担忧,需要辅助分析工具来调查故意添加的非法物质。带有电导检测的离子交换色谱法是一种用于测定各种基质中无机化合物的成熟分析技术。该技术已主要应用于杂质和降解产物的药物表征。这项工作提出了一种离子交换色谱法的新方法,作为一种筛选方法,用于调查宣传用于减肥的膳食补充剂中安非拉酮、非诺特罗、西布曲明、比沙可啶和阿米洛利的存在情况。该方法使用Metrosep C4 100/4.0阳离子交换柱进行了优化和验证。流动相由含2%乙腈(v/v)的1.8 mM硝酸组成,流速为0.9 ml/min,并采用非抑制电导检测。检测限和定量限分别在1.01至3.62 mg/L和1.48至8.72 mg/L之间。所提出的方法成功应用于78个固体膳食补充剂样品,其中两个样品发现掺假。此外,带有电导检测的离子交换色谱法无需事先进行复杂的样品预处理即可轻松用于质量控制。