Studies on Analytical Methods for N-Methylcarbamate Residues in Crops by Spectrophotometry and Gas Liquid Chromatography

작물체중(作物體中) N-Methylcarbamate계(系) 농약(農藥)의 잔류분석법(殘留分析法)에 관(關)한 연구(硏究)

Analytical methods for residues of six N-methylcarbamate insecticides were investigated to compare the minimum detectability, recovery from several crops and feasibility of multiple residue analysis. Those methods studied in this work included spectrophotometry by diazotization and gas chromatography by N-trifluoroacetylation(TFA), pentafluorobenzylether(PFB) and dinitrophenylether (DNP) derivatization. Maximum absorbed wavelength of the diazotized MIPC, XMC, BPMC, propoxur and carbofu ran was around 460 ㎚, while that of carbaryl recorded 510 ㎚. Recovery from brown rice and apple by diazotization method ranged from 80 to 120% and minimum detectable limits were 0.03 to 0.05 ppm in 50 g of the sample. Minimum detectability of PFB derivatives by gas chromatography was superior to TFA and DNP derivatives. DNP derivatives showed the longest retention time among the given derivatives. Recovery from crops by gas chromatographic met hod ranged 74 to 94%, 78 to 93%, and 85 to 99% in brown rice, rice straw and apple, respectively. Limit of detection was 0.01 ppm for TFA, 0.005 ppm for PFB and 0.02 ppm for DNP derivatives in 50 g of the crop samples.

N-Methylcarbamate계(系) 농약(農藥)의 잔류분석법(殘留分析法)을 확립(確立)하기 위하여 MIPC, XMC, BPMC, propoxur, carbofuran 및 carbary에 대하여 diazo화(化)에 의한 비색정량(比色定量)과 N-trifiuoroacetyl (TFA)화(化), pentafluorobenzyl ether(PFB)화(化) 및 dinitrophenyl ether (DNP)화(化)에 의한 유도체(誘導體)의 gas chromatography (ECD)法을 비교검토(比較檢討)하였다. 1) N-Methylcarbamate의 diazo화(化)에 의한 최대흡수파장(最大吸收波長)은 MIPC, XMC, BPMC, propoxur, carbofuran이 460 ㎚이었고 carbaryl은 510 ㎚이었다. 2) 비색법(比色法)에 의한 carbamate의 현미(玄米)와 사과중(中) 회수솔(回收率)은 명명(各各) $80{\sim}104%$, $98{\sim}120%$이었고, 50 g의 시료분석시(試料分析時) 최대검출한계(最大檢出限界)는 $0.03{\sim}0.05$ ppm의 범위(範圍)이었다. 3) Gas chromatography에 의한 carbamate의 분석(分析)에서는 DNP$0.01{\sim}0.2$ppm첨가시(添加時) 현미(玄米)에서 $74{\sim}94%$, 수도체(水稻體)에서 $78{\sim}93%$, 사과에서 $82{\sim}99%$의 범위(範圍)이었고 검출한계(檢出限界)는 50g의 시료분석시(試料分析時) TFA 0.01 ppm PFB 0.005ppm, DNP 0.01ppm이었다.