Department of Public Health and Community Medicine, Unit of Forensic Medicine, University of Verona, Verona, Italy.
J Chromatogr A. 2012 Dec 7;1267:198-205. doi: 10.1016/j.chroma.2012.08.085. Epub 2012 Sep 13.
For the first time a capillary separation based on micellar electrokinetic chromatography (MEKC) with diode array detection (DAD) was developed and validated for the rapid determination of synthetic cannabinoids in herbal blends. Separations were carried out on a 30 μm(ID) × 40 cm uncoated fused silica capillaries. The optimized buffer electrolyte was composed of 25 mM sodium tetraborate pH 8.0, 30 mM SDS and n-propanol 20% (v/v). Separations were performed at 30 kV. Sample injection conditions were 0.5 psi, 10s. Diazepam and JWH-015 were used as internal standards. The determination of the analytes was based on the UV signal recorded at 220 nm, corresponding to the maximum wavelength of absorbance of the molecules, whereas peak identification and purity check were also performed on the basis of the acquisition of UV spectra between 200 and 400 nm wavelengths. Under the described conditions, the separation of the compounds was achieved in 25 min without any significant interference from the matrix. Linearity was assessed within a concentration range from 5 to 100 μg/mL. The intra-day and inter-day imprecision values were below 2.45% for relative migration times and below 10.75% for relative peak areas. The present method was successfully applied to the direct determination of synthetic cannabinoids in 15 different herbal blend samples requiring only sample dilution. In addition, the developed MEKC separation was also applied to estimate the octanol/water partition coefficients (logP) of these new and poorly known molecules.
首次开发并验证了基于胶束电动色谱(MEKC)与二极管阵列检测(DAD)的毛细管分离方法,用于快速测定草药混合物中的合成大麻素。在 30μm(ID)×40cm 未涂层熔融石英毛细管上进行分离。优化的缓冲电解质由 25mM 硼酸钠 pH8.0、30mM SDS 和 20%(v/v)正丙醇组成。分离在 30kV 下进行。样品进样条件为 0.5psi、10s。安定和 JWH-015 用作内标。分析物的测定基于在 220nm 处记录的 UV 信号,这对应于分子的最大吸收波长,而峰识别和纯度检查也是基于在 200nm 至 400nm 波长范围内采集的 UV 光谱进行的。在所述条件下,在没有基质显著干扰的情况下,化合物在 25 分钟内实现分离。线性在 5 至 100μg/mL 的浓度范围内进行评估。日内和日间精密度值对于相对迁移时间低于 2.45%,对于相对峰面积低于 10.75%。该方法成功应用于 15 种不同草药混合物样品中合成大麻素的直接测定,仅需样品稀释。此外,所开发的 MEKC 分离还用于估计这些新的和知之甚少的分子的辛醇/水分配系数(logP)。