Paíga Paula, Rodrigues Manuela J E, Correia Manuela, Amaral Joana S, Oliveira M Beatriz P P, Delerue-Matos Cristina
REQUIMTE/LAQV, Instituto Superior de Engenharia do Instituto Politécnico do Porto, Rua Dr. António Bernardino de Almeida, 431, 4249-015 Porto, Portugal.
REQUIMTE/LAQV, Instituto Superior de Engenharia do Instituto Politécnico do Porto, Rua Dr. António Bernardino de Almeida, 431, 4249-015 Porto, Portugal; ESTiG, Instituto Politécnico de Bragança, Campus de Sta. Apolónia, 5300-253 Bragança, Portugal.
Eur J Pharm Sci. 2017 Mar 1;99:219-227. doi: 10.1016/j.ejps.2016.12.024. Epub 2016 Dec 24.
A method based on the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was successfully developed and validated for the analysis of 26 pharmaceutical compounds belonging to different therapeutic classes (anorexics, stimulants, anxiolytics, antidepressants and laxatives), which are all prone to be illegally added into weight-loss plant food supplements (PFS) for their pharmacological activity. Internal standard calibration with six isotopically labelled compounds rendered good linearity in the range of 5 to 1000μg/l, depending on the compound, and good sensitivity with limits of quantification in the range of 0.02-9.80μg/l. Recoveries were assessed for all the 16 samples analysed and were found between 70% and 120% for over 90% of the analytes. The average recovery value was 90.8%, for the different studied matrices (liquids, liquid ampoules, tablets and capsules), with RSD values lower than 10% for all forms. The changes introduced to the QuEChERS procedure maintained the good performance characteristics of the extraction method while preserving the chromatographic system for the introduction of unwanted matrix compounds. Synephrine was the only compound detected and quantified in one sample, but at a very low concentration (768μg/l) and its presence may be due to the plant extracts used in the formulation, as synephrine is known to be a natural constituent of Citrus aurantium amara. Despite none of the 16 evaluated samples were found to be adulterated by the illegal addition of the drugs included in this work, the developed methodology can be very useful for monitoring the adulteration of weight-loss PFS.
成功开发并验证了一种基于快速、简便、廉价、高效、耐用和安全（QuEChERS）萃取以及超高效液相色谱-串联质谱联用（UHPLC-MS/MS）的方法，用于分析26种属于不同治疗类别的药物化合物（食欲抑制剂、兴奋剂、抗焦虑药、抗抑郁药和泻药），这些药物都因其药理活性而容易被非法添加到减肥植物性食品补充剂（PFS）中。使用六种同位素标记化合物进行内标校准，根据化合物的不同，在5至1000μg/l范围内呈现出良好的线性，并且具有良好的灵敏度，定量限在0.02 - 9.80μg/l范围内。对所有分析的16个样品进行了回收率评估，发现超过90%的分析物回收率在70%至120%之间。对于不同的研究基质（液体、液体安瓿、片剂和胶囊），平均回收率值为90.8%，所有形式的相对标准偏差值均低于10%。对QuEChERS程序所做的更改保持了萃取方法的良好性能特征，同时保留了色谱系统以防止引入不需要的基质化合物。辛弗林是在一个样品中唯一检测和定量的化合物，但浓度非常低（768μg/l），其存在可能归因于制剂中使用的植物提取物，因为已知辛弗林是酸橙的天然成分。尽管在16个评估样品中均未发现因非法添加本研究中包含的药物而掺假，但所开发的方法对于监测减肥PFS的掺假可能非常有用。
