Astragalus Root, White Glabrous Greenbrier Rhizome And Root Of Herbaceous Peony Medicinal Herbs Pesticide Residue Measurement Method Research

Matrix solid-phase disperse GC and hollow fiber-based liquid phase microextraction GC were used to determine 20 organochlorine and pyrethroid pesticide residues in Radix astragali, Rhizoma Heterosmilax japonica, Radix paeoniae Alba..The conditions of matrix solid-phase disperse and hollow fiber-based liquid phase microextraction were optimized.Matrix solid-phase disperse GC was developed to determine 20 organochlorine and pyrethroid pesticide residues in Radix astragali, Rhizoma Heterosmilax japonica, Radix paeoniae Alba.The condition of matrix solid-phase disperse was optimized. The optimal condition was described as follows:the ratio of Chinese herbal medicine and florisil was 1:2,the ratio of water and florisil was 1:20 and the volume fraction of acetone in the petroleum ether-acetone mixed solution was 5%. Capillary column HP-5 (30 m×0.25 mm×0.25μm) was used. The detector was ECD. Inlet temperature was 230℃. The detector temperature was 280℃Column temperature: Carrying gas was nitrogen(1.0mL·min-1). Split ratio was 3:1. Volume was 1μL. GC method was applied for the determination of 20 organochlorine and pyrethroid pesticide residues in Radix astragali, Rhizoma Heterosmilax japonica, Radix paeoniae Alba.. The linear range for organochlorine pesticides was 5～500μg·L-1,the linear range for pyrethroid pesticides was 10～1000μg·L-1 (r=0.9979～0.9997). The mean recoveries in Radix astragali were 83.6%～110.3%,and the RSDs were 3.0%～9.9%.The mean recoveries in Rhizoma Heterosmilax japonica were 76.58 %～107.0%,and the RSDs were 3.0%～9.4%.The mean recoveries in Radix paeoniae Alba.were 82.9%～110.8%,and the RSDs were 2.9%～8.4%.The method was simple.It can be used for the determination of organochlorine and pyrethroid pesticide residues in Chinese herbal medicine.Hollow fiber-based liquid phase microextraction GC was developed to determine 20 organochlorine and pyrethroid pesticide residues in Radix astragali, Rhizoma Heterosmilax japonica, Radix paeoniae Alba..The condition of hollow fiber-based liquid phase microextraction was optimized. The optimal condition was described as follows:the extraction solvent was toluene,the stirring rate was 500 r·min-1 the concentration of NaCl was 10 mg·mL-1, the extraction time was 20 min.Capillary column HP-5 (30 m×0.25 mm×0.25μm) was used. The detector was ECD. Inlet temperature was 230℃. The detector temperature was 280℃. Column temperature: Carrying gas was nitrogen(1.0 mL·min-1). Split ratio was 3:1. Volume was 1μL. GC method was applied for the determination of 20 organochlorine and pyrethroid pesticide residues in Radix astragali, Rhizoma Heterosmilax japonica, Radix paeoniae Alba.. The linear range for organochlorine pesticides was 0.4～40μg·L-1,the linear range for pyrethroid pesticides was 0.8～80μg·L-1 (r =0.9970～0.9998).The mean recoveries in Radix astragali were 85.3%～109.4%,and the RSDs were 3.4%～9.2%.The mean recoveries in Rhizoma Heterosmilax japonica were 84.6 %～108.5%,and the RSDs were 2.8%～8.1%.The mean recoveries in Radix paeoniae Alba.were 85.4%～109.2%,and the RSDs were 3.6%～9.3%.The method was simple.It can be used for the determination of organochlorine and pyrethroid pesticide residues in Chinese herbal medicine.In this study, the results of the two methods are the same as the results with the application of sample pre-treatment method in "Chinese Pharmacopoeia" in 2005, and the pesticide types determined are more than the "Chinese Pharmacopoeia", in addition, the sample pre-treatment methods in this study are more simple,and less organic solvents were consumed.