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机构地区:[1]福建警察学院中心实验室,福建福州350007 [2]福建警察学院刑事科学技术系,福建福州350007
出 处:《福建分析测试》2010年第2期44-47,共4页Fujian Analysis & Testing
摘 要:本文研究了药丸中西地那非的高效液相色谱法鉴定。色谱柱为XDB-C18,5μm,4.6×150mm,二极管阵列检测器检测230nm(带宽4nm),流动相为35%乙睛+65%0.025mmol/L KH2PO4(含0.1‰v/v乙二胺)(pH5.57),流速1mL/min。样品用水溶解,外标法定量。检出限(LOD,S/N=3)为3μg/mL,定量限(LOQ,S/N=5)为4μg/mL。1000μg/mL、600μg/mL和200μg/mL的回收率分别为98.8%、101.3%和99.9%。6次测定600μg/mL和200μg/mL的相对标准偏差(RSD%)分别为2.4%和2.6%。在20~1000μg/mL范围内线型回归方程为Y=16.692X+50.17(Y为相应信号,mAU;X为浓度,μg/mL),回归系数R2为0.9998。该方法样品处理简单,定量准确度高,干扰小,可用于药丸中西地那非的法庭科学鉴定。Identification of sildenafil in suspected tablets by high Performance Liquid Chromatographic was investigated. Column stationary phase was XDB-C18, and a diode army detector monitored at 230nm with bandwidth 4nm. The mobile phase containing 35% acetonitril and 65% 0.025 mmol/L KH2PO4 added with 0.1‰ v/v diethylamine (pH5.57), flew at 1mL/min. Sample tablets were solved in water, and determined by external standard method. The limit of detection (LOD) of the method was 3 μ g/mL (S/N=3) and limit of quantification (LOQ) was 4 μ g/mL (S/N=5). Recoveries for 1000 μ g/mL,600 μ g/mL and 200 μ g/mL santdard solutions were 98.8%, 101.3% and 99.9% respectively. Relative standard deviations(RSD) for 600 μ g/mL and 200 μ g/mL standard solutions were 2.4% and 2.6%. In range of 20-10130 IS. g/mL linearity regression equation was Y=16. 69X+50.17(Y: response, mAU; X: concentration, μg/mL) with regressive coefficient(R^2)0.9998.Sample of the method is easily treated ,high accuracy of quantification and less disturbing ,it can be applied for identification of sildenafil in suspected tablets or capsules in forensic science cases.
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