海南益智中有机氯农药残留量的研究

Analysis of Organochlorine Pesticide Residue of Alpinia oxyphylla of Hainan

目的:建立气相色谱法测定中药材益智中有机氯(六六六,滴滴涕各4个异构体,五氯硝基苯及艾氏剂共10种)农药的残留量,同时测定海南道地益智中有机氯农药的残留量。方法:采用SE-54弹性石英毛细管(30 m×0.32 mm×25 μm)色谱柱,进样口温度为230℃;检测器温度为300℃。不分流进样,程序升温,检测器为63Ni电子捕获检测器,高纯氮气为载气。结果:10种有机氯农药在1-100 ng·mL-1范围内线性关系良好(r>0.9955),其检出限范围为0.05-0.23 ng·mL-1,定量限范围为0.20-0.72 ng·mL-1;益智中10种有机氯农药的回收率分别为101.1%,83.1%,84.9%,87.2%,97.0%,94.9%,99.5%,109.2%,90.1%及88.3%。结论:该方法的准确度、灵敏度、回收率及重现性均符合要求;同时,测定了海南道地益智中有机氯农药残留量,结果显示,海南不同产区益智的农残含量差异较大。

Objective:To analysis the content of organochlorine pesticide residue of Alpinia oxyphylla of Hainan. Methods: With gas chromatography(GC)and SE -54 flexible quartz capillary (30 m×0. 32 mm ×25μ m)chroma-tographic column, sample injection 230 ℃;63Ni electron capture detector (ECD); Detector temperature 300℃; Temperature programming. Results:10 kinds of organochlorine pesticide residue detected(4 isomers of 666,4 iso-mers of DDT,quintozene,drinox)of Alpinia oxyphylla had good linear correlation within 1 -100 ng·mL-1,the limit of detection was 0.05 - 0. 23 ng·mL-1, the limit of quantitation was 0. 20 - 0. 72 ng· mL-1; The recovery rate of 10 kinds of organochlorine pesticide residue was 101.1% ,83.1% ,84. 9% ,87. 2% ,97.0% ,94. 9% ,99. 5% , 109.2% ,90. 1% and 88. 3%. Conclusion: Organochlorine pesticide residue of Alpinia oxyphylla of Hainan varies greatly in different regions of Hainan. The content of organochlorine pesticide residue of Alpinia oxyphylla meets the green trade standard.