通过原位衍生化、固相微萃取和气相色谱-质谱联用技术测定水样中的抗炎药物。
Determination of anti-inflammatory drugs in water samples, by in situ derivatization, solid phase microextraction and gas chromatography-mass spectrometry.
作者信息
Araujo Lilia, Wild Johana, Villa Noreiva, Camargo Nuris, Cubillan Dalia, Prieto Avismelsi
机构信息
Laboratory of Analytical Chemistry and Electrochemistry, Faculty of Engineering, University of Zulia, P.O. Box 4011-A-526, Maracaibo, Venezuela.
出版信息
Talanta. 2008 Mar 15;75(1):111-5. doi: 10.1016/j.talanta.2007.10.035. Epub 2007 Oct 26.
A new analytical method for the determination of non-steroidal acidic anti-inflammatory drugs in water samples is described. These compounds are used as anti-inflammatory, antipyretic and analgesic drugs in human health care and in veterinary applications. Analytical procedure involves in situ derivatization of analytes to their methyl esters with dimethyl sulphate, headspace sampling using solid-phase microextraction (SPME), and gas chromatography-mass spectrometry (GC-MS). The effects of pH, ionic strength, extraction time, SPME fibre, extraction temperature as well as derivatization conditions were studied. Methyl esters were extracted with a fused-silica fibre coated with 100 microm polydimethylsiloxane. Response was linearly dependent on concentration in the range 0.1-10.0 ng mL(-1). Detection limits were achieved at the level of 0.3-2.9 ng L(-1). Derivatization-SPME/GC-MS analysis yielded good precision (R.S.D. between 7.9 and 17.2%). The method was validated by analysis of spiked matrix samples.
本文描述了一种用于测定水样中非甾体类酸性抗炎药的新分析方法。这些化合物在人类医疗保健和兽医应用中用作抗炎、解热和镇痛药。分析程序包括用硫酸二甲酯将分析物原位衍生化为其甲酯，使用固相微萃取（SPME）进行顶空采样，以及气相色谱-质谱联用（GC-MS）。研究了pH值、离子强度、萃取时间、SPME纤维、萃取温度以及衍生化条件的影响。用涂有100微米聚二甲基硅氧烷的熔融石英纤维萃取甲酯。响应在0.1 - 10.0 ng mL(-1)范围内与浓度呈线性相关。检测限达到0.3 - 2.9 ng L(-1)水平。衍生化-SPME/GC-MS分析具有良好的精密度（相对标准偏差在7.9%至17.2%之间）。该方法通过对加标基质样品的分析进行了验证。
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