合成大麻素JWH-250的高效液相色谱分析方法研究

Determination of Synthetic Cannabinoid JWH-250 by HPLC

目的建立合成大麻素JWH-250的高效液相色谱分析方法。方法考查梯度洗脱的有机相初始浓度和梯度洗脱的陡度、流速、柱温、检测波长等参数,初步建立JWH250的高效液相色谱分析方法,并对专属性、线性关系、精密度、稳定性等指标进行方法验证,进一步优化色谱条件,确定高效液相色谱法检测JWH-250的最佳条件。结果在紫外检测波长为214 nm,有机相初始浓度为63%,梯度陡度为4.2%/min,流速为0.8 m L/min,柱温34℃条件下,JWH-250在0.2~10μg/m L范围内线性良好,相关系数R=0.999 964 9,检出限（S/N≥3）为0.1μg/m L,日内精密度（RSD）为0.64%,日间精密度（RSD）为1.72%。结论实验表明,该方法测定合成大麻素JWH-250快速、灵敏、准确、可靠。

Objective As one kind of the most popular designer drugs, synthetic cannabinoid has been presenting a tough challenge for law enforcement and public security officials. JWH-250, one of the phenacyl-indoles abused all around the world, has recently been included under the latest Psychotropic Drug Directory by Chinese government. In order to improve the accuracy and sensitivity of determining JWH-250 in actual cases and enrich the research means for this drug, high performance liquid chromatography （HPLC） was utilized. Methods Chromatographic parameters were tested and optimized based on the performance of least interference to the results quality and repeatedness, together with the ascertainment of linear relationship, precision and stability. Eventually, the ideal conditions for detection of the synthetic cannabinoid JWH-250 by HPLC were established. Results Under optimized conditions （UV wavelength at 214 nm, initial concentration of the organic phase of 63%, gradient steepness of 4.2%/min, flow rate of 0.8 mL/min, and column temperature of 34℃）, a good linearity was achieved over the range of 2-100 μg/ml, with the correlation coefficient R=0.9999649 and limit of detection （ S/N ≥ 3 ） as to 0.1 μg/mL. The precision was good with the intra-day and inter-day RSDs less than 0.59% and 1.74%, respectively. JWH-250 can be completely separated from A9-tetrahydrocannabinol （THC）, cannabinol （CBN） and cannabidiol （CBD）. Conclusions The method is rapid, sensitive and accurate, applicable to quantitative determination of the synthetic cannabinoid JWH-250 by validation experiment of a sample from an actual case, a promising choice for providing technical support to prevent and combat the drug-related criminal activities,