Matrix Solid-phase Dispersion Extraction of Alkaloids from the Roots of Aconitum kusnezoffii Reichb

Matrix solid-phase dispersion（MSPD） was developed for the extraction of four alkaloids, including aconitine, mesaconitine, hypaconitine and deoxyaconitine, from the roots ofAconitum kusnezoffii Reichb. The determination of the analyte was carried out by high performance liquid chromatography with UV detection. The alkaline alumina was used as sorbent. The mixture of acetonitrile and water was used as elution solvent. Several extraction parameters, such as type of sorbent, the ratio of sample to solid support material, type of the elution solvent and the volume of the elution solvent were tested. Mean recoveries ranged from 93.16% to 102.73%, with relative standard deviations from 0.27% to 4.17%. With the extraction efficiency and time expenditure taken into account, MSPD extraction should be a comparatively good method.

多同位素内标气相色谱-质谱法测定食品中4种氯丙醇含量

采用多同位素内标法，结合七氟丁酰基咪唑（HFBI）衍生化的气相色谱-质谱（GC—MS）联用技术，建立了食品中4种氯丙醇含量的检测方法。对比了不同来源HFBI衍生试剂的作用性能，对定量内标物和校正标准的选择进行了比较。结果表明：仅用2种同位素内标（3．氯-1，2．丙二醇-d5（或2．氯．1，3．丙二醇．d，）和1，3．二氯．2．丙醇-d5）校正，同样可达到准确测定食品中4种氯丙醇含量的要求；若采用3-氯-1，2-丙二醇（3-MCPD）为标准物定量测定2-氯-1，3-丙二醇（2-MCPD）时，所得2-MCPD结果偏低，仅为以2．MCPD为标准物定量结果（真实值）的52．1％-77．8％。在最佳条件下进行了方法学指标的系统验证。4种氯丙醇的最低检出限为2．5～10gg／kg：在100-2000ng范围内，氯丙醇与内标物峰面积的比值和质量呈线性关系俾z〉0．9990）。以酱油和方便面调料粉为基质，进行100、200、4001xg／kg-1．个水平的加标回收实验，4种氯丙醇的回收率均值为90．1％～107％，相对标准偏差（RSD）为3．37％～10．4％（n=6），均满足痕量分析的要求。