Ribeiro Marcos Vinícius de Moura, Boralle Nivaldo, Felippe Lidiane Gaspareto, Pezza Helena Redigolo, Pezza Leonardo
Institute of Chemistry, São Paulo State University "Júlio de Mesquita Filho", 14800-060 Araraquara, SP, Brazil.
Institute of Chemistry, São Paulo State University "Júlio de Mesquita Filho", 14800-060 Araraquara, SP, Brazil.
Steroids. 2018 Oct;138:47-56. doi: 10.1016/j.steroids.2018.07.002. Epub 2018 Jul 10.
Counterfeiting and adulteration of pharmaceuticals is a prevalent problem worldwide and represents a major health risk to the population, with anabolic steroids being one of the main classes of drugs consumed and obtained from dubious sources. In this work, we propose the use of the H NMR technique to evaluate formulations containing anabolic steroids, with analysis of 40 samples of anabolic drugs that are used in injectable and capsule forms. The samples analyzed presented the following active ingredients: testosterone propionate, testosterone phenylpropionate, testosterone isocaproate, testosterone decanoate, testosterone cypionate, testosterone undecanoate, stanozolol, drostanolone propionate, trenbolone acetate, oxymetholone, and methandrostenolone. The H NMR spectroscopic measurements were performed using a 600 MHz Bruker Avance III spectrometer, with deuterated chloroform (CDCl) containing 0.1% TMS as solvent. Of the 40 samples analyzed, eight did not show the presence of the active principle stated on the label. Three types of adulteration were found in the analyzed samples: absence of the active ingredient, adulteration with other substances, and concentration values below those indicated on the label. Sildenafil citrate was found in four samples. The GC-MS technique was used to confirm the adulteration results found using H NMR. Quantitative determination by NMR was performed using internal standard and ERETIC 2 methods, and the results obtained were statistically the same.
药品的假冒和掺假是一个在全球普遍存在的问题，对民众构成重大健康风险，合成代谢类固醇是消费和从可疑来源获取的主要药物类别之一。在这项工作中，我们提议使用氢核磁共振技术来评估含有合成代谢类固醇的制剂，分析了40个用于注射剂和胶囊形式的合成代谢药物样本。所分析的样本含有以下活性成分：丙酸睾酮、苯丙酸睾酮、异己酸睾酮、癸酸睾酮、环戊丙酸睾酮、十一酸睾酮、司坦唑醇、丙酸屈他雄酮、醋酸群勃龙、羟甲烯龙和甲基雄烯醇酮。氢核磁共振光谱测量使用600兆赫的布鲁克Avance III光谱仪进行，以含有0.1%四甲基硅烷的氘代氯仿（CDCl）作为溶剂。在所分析的40个样本中，有8个未显示标签上所述活性成分的存在。在所分析的样本中发现了三种掺假类型：活性成分缺失、被其他物质掺假以及浓度值低于标签所示。在4个样本中发现了枸橼酸西地那非。使用气相色谱 - 质谱联用技术来确认通过氢核磁共振发现的掺假结果。通过核磁共振进行定量测定使用内标法和ERETIC 2方法，所获得的结果在统计学上是相同的。
