UFLC法测定新型“spike99”香料中JWH-073的含量

UFLC determination of the content of JWH-073 in "Spike99" spice

目的超快速液相色谱法测定新型"spike99"香料中JWH-073的含量。方法采用Shim-pack XR-ODSⅡ色谱柱(2.0mm×75mm,2.2μm);流动相:乙腈(含0.1%甲酸)∶水(含0.1%甲酸)(80∶20,v/v),流速:0.25mL/min;检测波长280nm,柱温:35℃,进样量:2μL,外标法定量测定JWH-073的含量。考查方法的线性范围、灵敏度、精密度、回收率和稳定性,并用于检测实际案例样品。结果 JWH-073浓度在1～50μg/mL范围内线性良好(A=9 398.7C-635.75,r=0.999 9);最低检测限为100ng/mL(S/N=3);低、中、高3种浓度的加样回收率(n=3)分别为100.52%(RSD=0.36%),99.52%(RSD=0.43%),99.03%(RSD=0.17%)。结论本法测定新型"spike99"香料中JWH-073含量操作简便、灵敏、准确,重复性好,适于在相关案件检验中选用。

Objective To establish an UFLC method for determination of the content of JWH-073 in new ＂spike99＂ spice.Methods Shim-pack XR-ODSⅡ chromatographic column（2.0mm×75mm,2.2μm） was used and the mobile phase consisted of acetonitrile and water（80∶20,v/v）,both eluents contained 0.1% formic acid.The mobile phase was pumped at a flow rate of 0.25mL/min.The UV detection wavelength was set at 280 nm.The column temperature was controlled at 35℃.The injection volume was 2μL.The content of JWH-073 in new type spice was calculated by external standardization method.The linearity range,sensitivity,precision,recovery and stability of this method were tested and could be used for detecting samples in real case.Results The calibration curve was linear with the range of 1~50μg/mL（A=9 398.7C-635.75,r=0.9999）.The detective limit was 100ng/mL（S/N=3）.The mean recoveries（n=3） of low,middle and high concentrations were 100.52%（RSD=0.36%）,99.52%（RSD=0.43%） and 99.03%（RSD=0.17%）,respectively.Conclusion A simple,selective,accurate and reproducible UFLC method was established for determination of JWH-073 content in new ＂spike99＂ spice and could be used in related cases.