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出 处:《分析测试学报》2014年第8期893-898,共6页Journal of Instrumental Analysis
基 金:公安部重点研究计划项目(201201ZDYJ005)
摘 要:建立了高效液相色谱法同时测定新型香料毒品中10种合成大麻素的分析方法.样品以甲醇提取,离心、过滤后,采用Shim-pack XR-ODS C18(4.6 mm×250 mm,5μm)色谱柱分离,以甲醇-乙腈(50>50)和水作为流动相进行梯度洗脱,柱温45℃,流速1.0 mL/min,检测波长220 nm.结果表明,该方法可在33 min内实现对常见10种合成大麻素的完全分离和定量,在1~100 mg/L线性范围内,相关系数均为0.999 9,检出限为0.10~0.50 mg/L.加标回收率为98.2%~102.1%,日内相对标准偏差(RSD)为0.15%~1.37%,日间相对标准偏差为0.55%~1.96%.样本在室温放置96 h、-20℃放置15 d以及在室温和-20℃反复冻融3次条件下稳定性均良好.该方法准确、快速、灵敏、分离效果好,适用于新型香料毒品中常见合成大麻素成分的检测.A high performance liquid chromatographic method was developed for the simultaneous determination of ten synthetic cannabinoids in novel "spice" drugs.A Shim-pack XR-ODS C18(4.6 mm× 250 mm,5 μm) column was used at 45 ℃.The mobile phase system contained methanol-acetonitrile(50 ∶ 50) and water,and the percentage of organic phase changed between 66%and 89.1% in a linear gradient elution.The flow rate was set at 1.0 mL/min,and the detection wavelength was 220 nm.Under the optimized conditions,ten synthetic cannabinoids were completely separated and determined in 33 min.Good linear relationships were obtained in the range of 1-100mg/L with correlation coefficients of 0.999 9.The LODs were in the range of 0.10-0.50 mg/L.The intra-day relative standard deviations(RSDs) were in the range of 0.15%-1.37% and the interday RSDs were 0.55%-1.96%.The sample showed good stability under room temperature,freeze and three cycles of freeze-thaw conditions.This method was accurate,sensitive and rapid for the determination of common synthetic cannabinoids in novel "spice" drugs.
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