HPLC-DAD法同时测定缴获毒品中曲马多、芬太尼和地芬诺酯的含量

HPLC-DAD Simultaneously Determining Tramadol, Fentanyl and Diphenoxylate in Seized Drugs

目的 建立了缴获毒品及非法添加的中草药样品中曲马多、芬太尼和地芬诺酯同时定量分析的高效液相色谱-二极管阵列(HPLC-DAD)检测方法。方法 样品经甲醇溶解超声提取后,采用Agilent Zorbax SBC18 (4.6mm×250mm, 5μm)色谱柱分离,12mmol/L磷酸二氢钾(10%稀磷酸调至pH=4)/乙腈梯度洗脱,在210nm波长下检测。结果 结果显示该3种待测成分检出限(S/N=3)在0.2~0.5μg/mL间、定量限(S/N=10)在0.5~1.0μg/mL间;在2~700μg/mL范围内线性关系良好,R2均大于0.999;黄色、白色粉末状毒品中三个浓度(所测样品原始含量的80%、100%、120%)平均加标回收率在99.6%~105.4%间,相对标准偏差(RSD%,n=6)小于1.4%;日间精密度在1.19%~2.11%间,重复性测试在0.31%~1.43%间,稳定性测试在0.29%~0.87%间。结论 该方法操作简单、准确,精密度、稳定性好,能够用于缴获毒品及非法添加的中草药样品中曲马多、芬太尼和地芬诺酯含量的定量分析。

Objective To establish an HPLC-DAD method for simultaneously quantitative analysis of tramadol, fentanyl and diphenoxylate in seized drugs and/or illegally-added herbal medicines. Methods The sample was dissolved into methanol and extracted under ultrasonic, having the obtained analytes separated through an Agilent Zorbax SB-C18(4.6×250mm, 5μm) column that was flowed with gradient-eluting of 12mM potassium dihydrogen phosphate buffer(pH=4 adjusted by 10% dilute phosphoric acid)/acetonitrile. The analysis was completed in 30 minutes and detected at the wavelength of 210nm. Results The three chemical substances were shown of their detection limits(S/N=3) and quantitation limits(S/N=10) among 0.2~0.5μg/mL and 0.5~1.0 μg/mL, respectively. The linear relationship was good in the range of 2~700μg/mL, with thecorrelation coefficients(R2) being all greater than 0.999, the three-concentration average recoveries(80%, 100%, 120%) in yellow and white powdery drugs among 99.6%~105.4%, the relative standard deviations(RSD%, n=6) being less than 1.4%, the inter-day precisions among 1.19%~2.11%, the repeatability within 0.31%~1.41%, and the stability being fallen into 0.29%~0.87%. Conclusions The method is simple, accurate, precise and stable, capable of quantitative analysis of tramadol, fentanyl and diphenoxylate in seized drugs and/or illegally-added herbal medicines.