Simultaneous determination of dichlorvos and trichlorfon in agricultural products by GC-FPD

被引:0
作者
Yamada, N [1 ]
Takahata, J [1 ]
Sasaki, K [1 ]
Toyoda, M [1 ]
Nakamura, R [1 ]
Yoshida, K [1 ]
机构
[1] Sendai City Inst Publ Hlth, Wakabayashi Ku, Sendai, Miyagi 9840002, Japan
来源
JOURNAL OF THE FOOD HYGIENIC SOCIETY OF JAPAN | 2002年 / 43卷 / 04期
关键词
dichlorvos; trichlorfon; agricultural products; derivatization; N-methylbis(trifluoroacetamide); method-performance study; interlaboratory study; repeatability; reproducibility;
D O I
10.3358/shokueishi.43.196
中图分类号
TS2 [食品工业];
学科分类号
0832 ;
摘要
We studied a gas chromatographic method for the determination of dichlorvos (DDVP) and trichlorfon (DEP) in agricultural products. DDVP and DEP were extracted from agricultural products with acetone and re-extracted with ethyl acetate instead of dichloromethane. DDVP and DEP were eluted in one fraction on a silica gel column using n-hexane-acetone (1 : 1). DEP is a thermally labile compound, so it was derived to a more thermally stable compound by acylation with N-methylbis(trifluoroacetamide) and pyridine in acetone at 60degrees\C for 2 hours. DDVP and the DEP-TFA derivative were determined simultaneously by GC-FPD. The recoveries of DDVP and DEP from agricultural products spiked at levels of 0.1 mug/g were 72.6similar to117.7% and 86.2similar to106.6%, respectively. The detection limits were 0.03 mug/g in powdered tea and less than or equal to0.01 mug/g in other samples. An interlaboratory study by 6 laboratories was conducted to validate this proposed method for 6 crops. Repeatability ranged from 3.1 to 7.8% for DDVP and from 3.4 to 8.3% for DEP, and reproducibility, from 6.9 to 15.5% for DDVP, and from 7.9 to 21.8% for DEP. Precision values were well within statistically predicted levels.
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页码:196 / 201
页数:6
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