School of Pharmacy, Qiqihar Medical University, Qiqihar 161006, China.
Molecules. 2018 Jun 21;23(7):1504. doi: 10.3390/molecules23071504.
The objective of this study was to establish a novel method for rapid detection of six glucocorticoids (prednisone, prednisone acetate, prednisolone, hydrocortisone, hydrocortisone acetate, and dexamethasone) added illegally in dietary supplements simultaneously by combining thin layer chromatography (TLC) with spot-concentrated Raman scattering (SCRS). The doping ingredients were separated by TLC, and viewed and located with UV light (254 nm), enriched by chromatography, then Raman spectra were directly detected by a Raman Imagine microscope with 780 nm laser source. This method had complementary advantages of TLC and Raman spectroscopy, which enhanced the specificity of the test results. The limit of detection (LOD) of the reference substances were 4 μg, 4 μg, 4 μg, 6 μg, 6 μg, and 4 μg, respectively. The method was used to study the six glucocorticoids added illegally in five dietary supplements. Fake drugs had been detected. The study showed that the TLC-SCRS method is simple, rapid, specific, sensitive, and reliable. The method could be used for effective separation and detection of six chemical components used in dietary supplement products, and would have good prospects for on-site qualitative screening of dietary supplement products for adulterants.
本研究旨在建立一种新的方法,用于快速检测同时添加到膳食补充剂中的六种糖皮质激素(泼尼松、醋酸泼尼松、泼尼松龙、氢化可的松、醋酸氢化可的松和地塞米松),该方法结合了薄层色谱(TLC)和斑点浓缩拉曼散射(SCRS)。掺杂成分通过 TLC 分离,用 254nm 的紫外光观察和定位,通过色谱富集,然后用 780nm 激光源的拉曼成像显微镜直接检测拉曼光谱。该方法具有 TLC 和拉曼光谱的互补优势,增强了测试结果的特异性。参考物质的检出限(LOD)分别为 4μg、4μg、4μg、6μg、6μg 和 4μg。该方法用于研究五种膳食补充剂中非法添加的六种糖皮质激素。已检测到假药。研究表明,TLC-SCRS 方法简单、快速、特异、灵敏、可靠。该方法可用于有效分离和检测膳食补充剂产品中使用的六种化学成分,有望对膳食补充剂产品中的掺杂物进行现场定性筛选。