Wu Wei, Ercal Nuran
Department of Chemistry, University of Missouri-Rolla, 1870 Miner Circle, Rolla, MO 65409, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Oct 5;809(2):295-9. doi: 10.1016/j.jchromb.2004.06.037.
Thiocyl (sodium thiosalicylate) belongs to a salicylate group of drugs, thus it has analgesic, antipyretic and anti-inflammatory effects. It possesses metal chelating function because it also belongs to a thiol-containing group of compounds which are well-known chelators. The studies of our research group showed that thiocyl is a promising chelator of lead poisoning due to its antioxidant and metal-chelating abilities. To the best of our knowledge, no methods were currently available for measuring thiocyl in biological samples. Therefore, we developed a reversed-phase HPLC method using fluorescence detection (lambdaex = 365 nm, lambdaem = 445 nm) with a one-step derivatizing reaction between thiocyl and a derivatizing agent-ThioGlo 3 (9-acetoxy-2-(4-(2, 5-dihydro-2,5-dioxo-1H-pyrrol-1-yl)pyenyl)-3-oxo-3H-naphtho[2,1-b]pyran). Most biological thiols (such as N-acetylcysteine (NAC), cysteine (CYS), glutathione (GSH) and homocysteine (HCYS)) do not interfere with the detection of thiocyl by using this technique. The linear range of its calibration curve was determined to be 25-2500 nM, and the detection limit of thiocyl was found to be 3 nM with 20 microL injection volume. The coefficients of variation (CV) for within-run precision and between-run precision ranged from 0.93 to 7.21%. This assay proved to be a rapid, sensitive and simple method for determining thiocyl in biological samples.
硫代水杨酸（硫代水杨酸钠）属于水杨酸类药物，因此具有镇痛、解热和抗炎作用。它具有金属螯合功能，因为它也属于含硫醇类化合物，而这类化合物是众所周知的螯合剂。我们研究小组的研究表明，硫代水杨酸因其抗氧化和金属螯合能力，是一种有前景的铅中毒螯合剂。据我们所知，目前尚无测定生物样品中硫代水杨酸的方法。因此，我们开发了一种反相高效液相色谱法，采用荧光检测（激发波长λex = 365 nm，发射波长λem = 445 nm），硫代水杨酸与衍生化试剂硫代荧光素3（9 - 乙酰氧基 - 2 - （- 4 - （2,5 - 二氢 - 2,5 - 二氧代 - 1H - 吡咯 - 1 - 基）苯基） - 3 - 氧代 - 3H - 萘并[2,1 - b]吡喃）之间进行一步衍生化反应。使用该技术，大多数生物硫醇（如N - 乙酰半胱氨酸（NAC）、半胱氨酸（CYS）、谷胱甘肽（GSH）和同型半胱氨酸（HCYS））不会干扰硫代水杨酸的检测。其校准曲线的线性范围确定为25 - 2500 nM，进样体积为20 μL时，硫代水杨酸的检测限为3 nM。批内精密度和批间精密度的变异系数（CV）范围为0.93%至7.21%。该测定方法被证明是一种快速、灵敏且简单的测定生物样品中硫代水杨酸的方法。
