Institute of Chinese Medical Sciences, University of Macau, Taipa, Macao SAR, P. R. China.
J Sep Sci. 2011 Dec;34(23):3372-82. doi: 10.1002/jssc.201100712. Epub 2011 Oct 20.
A fast gas chromatography coupled with mass spectrometry (GC-MS) using large volume injection with programmed temperature vaporizer in solvent vent mode (PTV-LVI-SV) was developed for the trace determination of multiple pesticide residues in traditional Chinese medicines (TCMs). Experimental conditions of PTV-LVI-SV injection were optimized by central composite design. The optimized result was that initial temperature was held at 40°C for 39 s, vent flow rate was set at 45 mL/min and vent pressure was held at 0 psi for 36 s, injection volume was 10 μL. Furthermore, the quick and effective QuEChERS (quick, easy, cheap, effective, rugged and safe) method was performed to extract and purify pesticide residues in TCMs. The prepared samples were analyzed with GC-MS in the selected ion monitoring mode (SIM). The lowest LOD was 4 μg/kg for some pesticides. The recoveries were checked by spiking samples with pesticides at 25, 50 and 250 μg/kg. The average recoveries of most pesticides were from 80 to 118%. The result indicated that QuEChERS and PTV-LVI-SV GC-MS method was a rapid and sensitive analysis technique for the determination of multiple pesticide residues in TCMs.
建立了一种快速气相色谱-质谱联用技术（GC-MS），采用程序升温汽化进样-溶剂解吸模式（PTV-LVI-SV），结合大体积进样，用于测定中药材中多种农药残留。通过中心组合设计优化了 PTV-LVI-SV 进样的实验条件。优化结果为：初始温度保持在 40°C 39 s，解吸气流速度设定为 45 mL/min，解吸压力保持在 0 psi 36 s，进样量为 10 μL。此外，采用快速、简便、廉价、有效、耐用和安全（QuEChERS）方法提取和净化中药材中的农药残留。用选择离子监测模式（SIM）的 GC-MS 对制备的样品进行分析。部分农药的最低检出限为 4 μg/kg。通过在 25、50 和 250 μg/kg 水平下向样品中添加农药进行回收率检查。大多数农药的平均回收率在 80%至 118%之间。结果表明，QuEChERS 和 PTV-LVI-SV GC-MS 方法是一种快速、灵敏的分析技术，可用于测定中药材中的多种农药残留。
