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A new approach to ion exchange chromatography with conductivity detection for adulterants investigation in dietary supplements

机译:膳食补充剂掺杂剂对掺杂剂检测的一种新方法

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Abstract 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?m m HNO 3 containing 2% acetonitrile (v/v), with a flow rate of 0.9?ml?min ?1 , and nonsuppressed conductivity detection was applied. The limits of detection and quantification varied from 1.01 to 3.62?mg?L ?1 and from 1.48 to 8.72?mg?L ?1 , 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.
机译:摘要近年来膳食补充剂掺假程度显着增加。这种情况担忧卫生当局并要求辅助分析工具进行专动添加的非法物质。具有电导率检测的离子交换色谱是一种综合分析技术,用于测定各种基质中的无机化合物。该技术已应用于主要杂质和降解产物的药物表征。该工作呈现了一种新的离子交换色谱法作为筛选方法,以研究Amfepramone,Femproporex,Sibutramine,双育odyl和氨基甲酰的饮食补充剂中的筛选方法,该方法为减肥造成的膳食补充剂。使用MetroSEP C4 100 / 4.0阳离子交换柱进行优化和验证该方法。流动相由含有2%乙腈(v / v)的1.8·m m HnO 3组成,流速为0.9≤ml≤1,并施加非卷积电导率检测。检测和定量的限制分别从1.01到3.62?mg?1和1.48至8.72Ωmg?1。该方法成功地应用于78个固体膳食补充剂样品,其中在其中发现掺杂剂。此外,具有电导检测的离子交换色谱可以容易地用于质量控制,而无需现有的复杂样品预处理。

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