采用GC法测定天然冰片中的d-龙脑和樟脑的含量。分析柱为CP-WAX毛细管柱<30 m×0.32 mm×0.5μm>;升温程序为50℃,以5℃/min升温到100℃,保持1 min,再以10℃/min快速升温到180℃,保持5 min,进样流速比5∶1;FID检测器温度...采用GC法测定天然冰片中的d-龙脑和樟脑的含量。分析柱为CP-WAX毛细管柱<30 m×0.32 mm×0.5μm>;升温程序为50℃,以5℃/min升温到100℃,保持1 min,再以10℃/min快速升温到180℃,保持5 min,进样流速比5∶1;FID检测器温度为250℃;进样口温度为200℃,载气为高纯氮气,体积流量为2 m L/min;空气体积流量为300 m L/min;氢气体积流量为30 m L/min;进样量为1μL。本方法操作简便、准确,精密度、分离度良好、分析时间短,为天然冰片的测定及其质量控制提供参考。展开更多
A rapid method was developed for the determination of 22 pesticides in rice wine. The procedure involved an extraction with acetonitrile and a cleanup step using dispersive solid-phase extraction (d-SPE), and primary-...A rapid method was developed for the determination of 22 pesticides in rice wine. The procedure involved an extraction with acetonitrile and a cleanup step using dispersive solid-phase extraction (d-SPE), and primary-secondary amine (PSA) and octadecylsilane (ODS) were used as sorbents. D-SPE had some advantages over some traditional prepara- tions, especially in time and cost. Both the extraction and cleanup only cost about 15 min per a sample. Then the GC-MS was used for quantitative and qualitative analysis. Matrix-matched standards solution and analyte protectant were compared to decrease the matrix effect, and the former showed a better efficacy. Acceptable linearity was achieved in the range of 0.05 - 0.30 mg/L. After matrix-matched standards calibration, recoveries were between 60 and 140%. For the most of pesticides, precision and repeatability were less than 10% and 16%, respectively. The result indicated that the developed method was suitable for the determination of the multi-pesticides in rice wine.展开更多
文摘采用GC法测定天然冰片中的d-龙脑和樟脑的含量。分析柱为CP-WAX毛细管柱<30 m×0.32 mm×0.5μm>;升温程序为50℃,以5℃/min升温到100℃,保持1 min,再以10℃/min快速升温到180℃,保持5 min,进样流速比5∶1;FID检测器温度为250℃;进样口温度为200℃,载气为高纯氮气,体积流量为2 m L/min;空气体积流量为300 m L/min;氢气体积流量为30 m L/min;进样量为1μL。本方法操作简便、准确,精密度、分离度良好、分析时间短,为天然冰片的测定及其质量控制提供参考。
文摘A rapid method was developed for the determination of 22 pesticides in rice wine. The procedure involved an extraction with acetonitrile and a cleanup step using dispersive solid-phase extraction (d-SPE), and primary-secondary amine (PSA) and octadecylsilane (ODS) were used as sorbents. D-SPE had some advantages over some traditional prepara- tions, especially in time and cost. Both the extraction and cleanup only cost about 15 min per a sample. Then the GC-MS was used for quantitative and qualitative analysis. Matrix-matched standards solution and analyte protectant were compared to decrease the matrix effect, and the former showed a better efficacy. Acceptable linearity was achieved in the range of 0.05 - 0.30 mg/L. After matrix-matched standards calibration, recoveries were between 60 and 140%. For the most of pesticides, precision and repeatability were less than 10% and 16%, respectively. The result indicated that the developed method was suitable for the determination of the multi-pesticides in rice wine.
