气相色谱法测定茶叶中八氯二丙醚(S-421)残留量
Gas-Chromatographic Determination of Residual Octachloro-Dipropyl-Ether (S-421) in Tea
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摘要: 建立了一种测定茶叶中八氯二丙醚(S-421)残留量的气相色谱方法.试样中的八氯二丙醚(S-421)经丙酮提取、正己烷反萃取,然后用浓硫酸液-液分配磺化法,进行净化,以气相色谱法(GC-ECD)测定,外标法定量.试验结果表明:试样中加入0.005~0.05 mg·kg-1浓度水平的八氯二丙醚(S-421),回收率在85%~110%,检出限为0.005 mg·kg-1.同一样品10次测定的相对标准偏差小于10%.Abstract: The residual octachloro-dipropylether (S-421) in tea was extracted with acetone and back-extracted with n-hexane.The S-421 in n-hexane was cleaned by liquid-liquid partition sulfonation with conc.H2SO4,and the sulfonated S-421 in n-hexane was used for GC determination.Measurements were made by ECD,and the method of external standards was use in determination.Tests of recovery were made by addition of standard S-421 to several portions of a tea sample at the concentration levels in the range of 0.005-0.05 mg·kg-1,and the values of recovery found were in the range of 85%-110%.Detection limit of the present method was 0.005 mg·kg-1.Precision of the method was tested by analyzing a same sample for 10 determinations,the values of RSD′s found were less than 10%.