Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia; Department of Chemistry, Faculty of Science, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Dec 1;940:59-65. doi: 10.1016/j.jchromb.2013.09.017. Epub 2013 Sep 23.
Mesoporous silica material, MCM-41, was utilized for the first time as an adsorbent in solid phase membrane tip extraction (SPMTE) of non-steroidal anti-inflammatory drugs (NSAIDs) in urine prior to high performance liquid chromatography-ultraviolet (HPLC-UV) analysis. The prepared MCM-41 material was enclosed in a polypropylene membrane tip and used as an adsorbent in SPMTE. Four NSAIDs namely ketoprofen, diclofenac, mefenamic acid and naproxen were selected as model analytes. Several important parameters, such as conditioning solvent, sample pH, salting-out effect, sample volume, extraction time, desorption solvent and desorption time were optimized. Under the optimum extraction conditions, the MCM-41-SPMTE method showed good linearity in the range of 0.01-10μg/mL with excellent correlation coefficients (r=0.9977-0.9995), acceptable RSDs (0.4-9.4%, n=3), good limits of detection (5.7-10.6μg/L) and relative recoveries (81.4-108.1%). The developed method showed a good tolerance to biological sample matrices.
介孔硅材料 MCM-41 首次被用作固相膜探头萃取（SPMTE）的吸附剂，用于尿液中非甾体抗炎药（NSAIDs）在高效液相色谱-紫外（HPLC-UV）分析之前的提取。制备的 MCM-41 材料被封装在聚丙膜探头中，并用作 SPMTE 的吸附剂。选择了四种 NSAIDs，即酮洛芬、双氯芬酸、甲芬那酸和萘普生作为模式分析物。优化了几个重要参数，如调节溶剂、样品 pH 值、盐析效应、样品体积、萃取时间、洗脱溶剂和洗脱时间。在最佳萃取条件下，MCM-41-SPMTE 方法在 0.01-10μg/mL 范围内具有良好的线性，相关系数优秀（r=0.9977-0.9995），可接受的 RSD（0.4-9.4%，n=3），良好的检测限（5.7-10.6μg/L）和相对回收率（81.4-108.1%）。该方法对生物样品基质具有良好的耐受性。
