中药材中氨基甲酸酯类农药残留量的反相高效液相色谱法  

RP -HPLC Determination of Residual Amount of Aldicarb, Carbofuran and Carbaryl in Chinese Crude Drugs

作　　者：董顺玲[1] 胡家炽[1] 何志强[1] 杨仲元[1] 

机构地区：[1]广州市药品检验所,广州510160

出　　处：《药物分析杂志》2002年第3期178-182,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家中医药管理局科学基金(95B142)

摘　　要：目的:测定三七、西洋参、白芍和当归中涕灭威、呋哺丹、西维因3种氨基甲酸酯农药残留量。方法:用丙酮超声波提取,二氯甲烷液液分配萃取,中性氧化铝层析柱(25cm×1.5 cm)净化,采用YWG-C_(18)色谱柱(250mm×4.6 mm,5μm),以乙腈-水(38:62)为流动相,流速为1.0 mL·min^(-1),检测波长分别为200nm(检测涕灭威、 呋喃丹)和220nm(检测西维因);检测浓度分别为:涕灭威0.52μg·mL^(-1) ,呋喃丹0.40μg·mL^(-1) ,西维因0.11μg·mL^(-1);进样量为20μL。结果:涕灭威、呋喃丹、西维因添加回收率分别为83.1％～91.5％,90.1％～110.6％,94.0％～96.9％;RSD分别为3.5％～8.0％,1.9％～7.6％,2.9％～6.3％;检测限(S/N=3)分别为:涕灭威2.4×10^(10)g,呋喃丹8.4×10^(-11)g,西维因4.4×10^(11)g。结论:本方法分离净化效果好,选择性强,灵敏度高,操作简便等。Objective: To determine the residues of aldicarb, carbofuran and carbaryl in Panax notoginseng (BurK. ) F. H. Chen, Panax quinguefolium L. , Paeonia lactiflora Pall. and Angelica sinensis (Oliv. ) Diels. Method: The samples were extracted with acetone, purification of the pesticides was performed using a column (25 cm × 1. 5 cm) packed with 10 g Al2O3 ( contain 3. 0% water) . The RP - HPLC was conducted with a YWG - C18 (250 mm ×4. 6 mm 5 μm) column, acetonitrile - water (38: 62) as mobile phase, flow rate was 1. 0 mL·min-1 ; 200 nm (for aldicarb, carbofuran) and 220 nm (for carbaryl) as detection wavelengths, the detection concentration was : 0. 52, 0. 40, 0.11 μg ·mL-1 respectively and the injection volume was 20 μL. Results: The recoveries of aldicarb, carbofuran and carbaryl were 83. 1% - 91. 5% , 90. 1% - 110.6% , 94.0% -96. 9% , respectively. Corresponding RSDs were 3. 5% - 8. 0% , 1.9% - 7. 6% , 2. 9% - 6. 3% , respective-ly. The detection limits (S/N = 3) were 2. 4×10-10, 8.4×10-11, 4. 4×10-11g, respectively. Conclusion: This method is sensitive, selective and easy for operation.

关 键 词：中药材 氨基甲酸酯类 农药残留量 反相高效液相色谱法 

分 类 号：R288[医药卫生—中药学] S481.8[医药卫生—中医学]