高效薄层色谱法（HPTLC）分析农药残留
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摘要
本文以呋喃丹、西维因、抗蚜威和灭多威等4种氨基甲酸酯与溴氰菊酯、甲氰菊酯和联苯菊酯等3种拟除虫菊酯杀虫剂作为供试农药，探讨了应用高效薄层色谱法(HPTLC)分析农药残留的方法，研究了影响分离与检测的主要因素，并应用HPTLC方法检测了几种蔬菜中7种农药残留。主要研究结果如下：
1．在常温(4-20℃)与通常的湿度(50％-100％)下，采用上行展开，筛选了单种和混合农药的展开系统。
单种农药展开系统，抗蚜威与灭多威用甲苯-丙酮(7：3，v／v)展开，R_f值为0.66和0.37，用石油醚-乙酸乙酯(5：5，v／v)展开，R_f值分别为0.76和0.44；呋喃丹与西维因以二氯甲烷-甲苯-乙酸乙酯(8：1：1，v／v)作为展开系统，R_f值分别达0.48和0.63，而用氯仿展开时，R_f值分别为0.25和0.50；应用甲苯展开溴氰菊酯与甲氰菊酯，R_f值依次为0.77和0.63，在以环已烷-氯仿(5：5，v／v)作为另一种展开系统时，R_f值分别为0.47和0.40；联苯菊酯的两种展开系统分别是甲苯-石油醚(5：5，v／v)(R_f值0.73)和环已烷-氯仿(8：2，v／v)(R_f值0.54)；这些展开系统为筛选、优化混和农药的展开方法奠定了基础，也可作为单残留检测及确证的依据。
抗蚜威、灭多威、西维因和呋喃丹等4种氨基甲酸酯杀虫剂的展开方法Ⅰ_(car)，先用甲苯-丙酮(8：2，v／v)展开45mm，再用二氯甲烷-甲苯(8：2，v／v)展到70mm；展开方法Ⅱ_(car)，先用乙酸乙酯-石油醚(6：4，v／v)展开35mm，再用氯仿-石油醚(8：1，v／v)展开70mm。溴氰菊酯、甲氰菊酯和联苯菊酯等3种拟除虫菊酯类混合农药的展开方法Ⅰ_(pyr)是用甲苯-石油醚(8：3，v／v)展70mm；展开方法Ⅱ_(pyr)用环已烷-氯仿(5：5，v／v)展70mm。应用展开方法Ⅰ_(car)与Ⅰ_(pyr)，抗蚜威与灭多威、呋喃丹与西维因、甲氰菊酯与溴氰菊酯的分离度分别为2.36，1.56，1.17，均优于展开方法Ⅱ_(car)与Ⅱ_(pyr)，尤其是在Ⅱ_(pyr)下甲氰菊酯与溴氰菊酯的分离度为0.78＜1.0，分离不理想。以展开方法Ⅰ_(car)与Ⅰ_(pyr)为筛选体系，用于样品提取中残留农药筛选检测，而以展开方法Ⅱ_(car)与Ⅱ_(pyr)作为确证系统，用于初检中呈阳性样品的复检及确证。
2．影响HPTLC对7种农药分离和定量测定的主要因素表现为：
在4s／ul～15s／ul的点样速度范围内，分别点样20ng、50ng、100ng、200ng和300ng，检测结果表明，用15s／uL，的点样速度得出的峰高依次为4s／uL的2.9、2.6、1.5、1.3和1.1倍；因此点样速度慢有利于定量。但长时间的点样过程，使活化后的干燥的薄层吸附空气中的水汽的机会增多，不利于湿度要求严格的展开剂展开，综合比较以10s／ul点样速度比较适宜；
点样带宽对定量与分离均有影响，20ng、50ng、100ng、200ng和300ng等5种点样量，随带宽从1mm增大到10mm，其峰高从194.2～382.9AU降低到106.3～326.3AU，对分离影响最显著的是抗蚜威与灭多威，其分离度随带宽由3mm增大到10mm而增加了1.3倍。而蔬菜杂质较多，既需要农药之间很好地分
离，又需要农药与杂质分开，故选取6mm带宽。
展开湿度：研究了 9％、14％、18％、32％、42％、47％、65％、72％及大于
72％等9种湿度下的分离与定量效果，结果表明，应用展开方法Ic。r，在湿度大
于 72％时4种氨基甲酸酯分离最好，而 3种拟除虫菊酯在展开方法 I叮r下的分离
则几乎不受湿度影响，但其定量有差异，300ng点样量9％湿度下峰高为65％的
l．5倍左右。
温度对农药的分离影响不大，但对定量有影响，300ng／斑点4OC下所测得峰
高为 30C下的 1．01～l．23倍。
扫描狭缝的大小直接影响着定量，实验表明：物质最灵敏的扫描狭缝大小总
是小于其点样带宽的大小，并且狭缝的长度比宽度影响要大，当带宽为4与smm
时，样品展开后，用 2．00 X 0．20mm的狭缝扫描的峰高与峰面积均最大，6mm带宽
则用 4．00 X 0．30mm的狭缝最灵敏。
3．最小检测量和方法精密度。7种农药的最小检测限分别为西维因：Zng；味
哺丹、抗蚜威、灭多威、涣氰菊酯、甲氰菊酯与联苯菊酯均为 10ng；定量限分别
为4种氨基甲酸酯30ng，3种拟除虫菊酯20ng。50ng含量农药在上述展开方法
1展开后，无论是薄层扫描仪的精密度，还是包括点样精密度、簿层均匀度及展
开后有无边缘效应等的方法精密度，都是以峰高作为定量依据优于以峰面积作为
定量依据，对于上述7种农药，以峰高作为定量依据，薄层扫描仪检测相对标准
偏差（RSD）是在 1．07％－3．96％，方法 RSD在 3．61％－10．94％。
4．以马铃薯、冬瓜、青菜、空心菜、大豆和豆角等6种蔬菜为对象，分别建
立了4种氨基甲酸酯、3种拟除虫菊酯杀虫剂的HPTLC残留分析方法。实验表明：
由于蔬菜基质中杂质的影响，需对展开方法进行调整。
4种氨基甲酸酯杀虫剂的展开方法，Ic。r相应调整为在常温与大于 72％湿度
下上行展开，先用甲苯－丙酮（8：2，V八）展45VV，再用二氯甲烷－甲苯（：2，V灯）展
80mm，最后用二氯甲烷展到 80mm；11帕r被在 18％湿度下水平展开，先用二氯甲
烷－丙酮四：l，v／v）展 35mm，再用二氯甲烷展到 80mm代替。s种拟除?
In this paper, studies were conducted to determination the residues of pirimicarb, methomyl, carbaryl, carbofuran, fenpropathrin, deltamethrin and bifenthrin in vegetables with high-performance thin-layer chromatography(HPTLC). The factors that affected the determination were further investigated. The main results were summarized as following:
1. Two mobile phases were selected in two-trough chamber under normal temperature(4-20癈) and humidity (50-100%) for separating the pesticides standard. If mobile phase was toluene-acetone(7:3,v/v), the Rf valve of pirimicarb and methomyl were 0.66 and 0.37, while the Rf were 0.76 and 0.44 with petroleum ether-acetate ethyl(5:5,v/v). The first of carbofuran and carbaryl was dichloromethane-toluene-acetate ethyl(8:1:1,v/v) with the Rfof 0.48 and 0.63, and second was chloroform with the Rfof 0.25 and 0.50. The mobile phases of deltamethrine and fenpropathrin were toluene (0.77 and 0.63), and cyclohexane-chlorofornn (5:5,v/v) ( 0.47 and 0.40). Bifenthrin could be developed with toluene-petroleum ether (5:5,v/v) and cyclohexane-chloroform(8:2,v/v) respectively, the corresponding Rfwere 0.73 and 0.54 . All the mobile phases for single pesticides provide a theoretical base for mixed pesticides.
For 4 carbamates, the first system ( I car) was toluene-acetone(8:2,v/v) and dichloromethane-acetone(8:2,v/v). The migration distances were 45mm and 70mm respectively. Second one(IIcar) was petroleum ether- ethyl acetate (4:6,v/v) with 35mm, and then petroleum ether-chloroform (9:1,v/v) with 70mm.Toluene-petroleum ether(8:3,v/v) was system I pyr for 3 pyrethroids. And II pyr was cyclohexane -chloroform(5:5, v/v). The migration distances are both 70mm. Since the resolution (R) of pirimicarb and methomyl, carbofuran and carbaryl, fenpropathrin and deltamethrin, are 2.36,1.56,1.17 with mobile phase I car and I pyr, which are superior to that of II car and II pyr Especially separation of fenpropathrin and deltamethrin was not idea for 0.87 with II pyr So the former two were for quantification, the latter two were for qualification if they would work well in vegetables.
2. The factors that affected the determination:
When the speed of sample injection was within the range of 4s/ul to 15s/ul, the peak heights of contents of 20,50,100,200 and 300ng with 15s/ul were higher than that of 4s/ul by 2.9,2.6,1.5,1.3 and 1.1 times respectively. While the long time spent in the sample injection make the chances that thin-layer after activation absorbed vapour in air increased. 10s/ul was proper according to its time and effect.
The quantification and separation of pesticides were also affected by the band. For the contents of 20,50,100,200 and 300ng, the peak heights of them were194.2-382.9AU
with the band of 1mm , decreasing to106.3~326.3AU with that of 10mm. The separation of pirimicarb and methomyl was affected greatly by the band. R increased by 1.3 times when the band was from 3mm to 10mm. The band also affected the separation of 3 pyrethroids and impurity in spiked green vegetables. So 6mm was selected as the band width of sample injection.
Among the humidity of 9%, 14%, 18%, 32%, 42%, 47%, 65%, 72% and over 72%, 4 carbamates were separated best with mobile phase I Car in the humidity of over 72%, and the separation effect of 3 pyrethroids was not affected by humidity with I pyr, while the quantification was related to humidity. The peak heights of SOOng content of pyrethroids after development in the humidity of 9% were more than that in 65% by 1.5 times.
Studies also manifested that the peak heights of 300ng content after development in 4'C were 1.01 to 1.23 times as that in 30℃, while separation of 7 pesticides were good in both temperature.
The scanner slit was a main factor to determination. Results showed that the favourable scanner slit was always smaller than the band of sample injection, and the length was more important than the width of the scanner slit. When the band was 4mm or 5mm after development, the slit of 2.00×0.20mm was idea.
1．在常温(4-20℃)与通常的湿度(50％-100％)下，采用上行展开，筛选了单种和混合农药的展开系统。
单种农药展开系统，抗蚜威与灭多威用甲苯-丙酮(7：3，v／v)展开，R_f值为0.66和0.37，用石油醚-乙酸乙酯(5：5，v／v)展开，R_f值分别为0.76和0.44；呋喃丹与西维因以二氯甲烷-甲苯-乙酸乙酯(8：1：1，v／v)作为展开系统，R_f值分别达0.48和0.63，而用氯仿展开时，R_f值分别为0.25和0.50；应用甲苯展开溴氰菊酯与甲氰菊酯，R_f值依次为0.77和0.63，在以环已烷-氯仿(5：5，v／v)作为另一种展开系统时，R_f值分别为0.47和0.40；联苯菊酯的两种展开系统分别是甲苯-石油醚(5：5，v／v)(R_f值0.73)和环已烷-氯仿(8：2，v／v)(R_f值0.54)；这些展开系统为筛选、优化混和农药的展开方法奠定了基础，也可作为单残留检测及确证的依据。
抗蚜威、灭多威、西维因和呋喃丹等4种氨基甲酸酯杀虫剂的展开方法Ⅰ_(car)，先用甲苯-丙酮(8：2，v／v)展开45mm，再用二氯甲烷-甲苯(8：2，v／v)展到70mm；展开方法Ⅱ_(car)，先用乙酸乙酯-石油醚(6：4，v／v)展开35mm，再用氯仿-石油醚(8：1，v／v)展开70mm。溴氰菊酯、甲氰菊酯和联苯菊酯等3种拟除虫菊酯类混合农药的展开方法Ⅰ_(pyr)是用甲苯-石油醚(8：3，v／v)展70mm；展开方法Ⅱ_(pyr)用环已烷-氯仿(5：5，v／v)展70mm。应用展开方法Ⅰ_(car)与Ⅰ_(pyr)，抗蚜威与灭多威、呋喃丹与西维因、甲氰菊酯与溴氰菊酯的分离度分别为2.36，1.56，1.17，均优于展开方法Ⅱ_(car)与Ⅱ_(pyr)，尤其是在Ⅱ_(pyr)下甲氰菊酯与溴氰菊酯的分离度为0.78＜1.0，分离不理想。以展开方法Ⅰ_(car)与Ⅰ_(pyr)为筛选体系，用于样品提取中残留农药筛选检测，而以展开方法Ⅱ_(car)与Ⅱ_(pyr)作为确证系统，用于初检中呈阳性样品的复检及确证。
2．影响HPTLC对7种农药分离和定量测定的主要因素表现为：
在4s／ul～15s／ul的点样速度范围内，分别点样20ng、50ng、100ng、200ng和300ng，检测结果表明，用15s／uL，的点样速度得出的峰高依次为4s／uL的2.9、2.6、1.5、1.3和1.1倍；因此点样速度慢有利于定量。但长时间的点样过程，使活化后的干燥的薄层吸附空气中的水汽的机会增多，不利于湿度要求严格的展开剂展开，综合比较以10s／ul点样速度比较适宜；
点样带宽对定量与分离均有影响，20ng、50ng、100ng、200ng和300ng等5种点样量，随带宽从1mm增大到10mm，其峰高从194.2～382.9AU降低到106.3～326.3AU，对分离影响最显著的是抗蚜威与灭多威，其分离度随带宽由3mm增大到10mm而增加了1.3倍。而蔬菜杂质较多，既需要农药之间很好地分
离，又需要农药与杂质分开，故选取6mm带宽。
展开湿度：研究了 9％、14％、18％、32％、42％、47％、65％、72％及大于
72％等9种湿度下的分离与定量效果，结果表明，应用展开方法Ic。r，在湿度大
于 72％时4种氨基甲酸酯分离最好，而 3种拟除虫菊酯在展开方法 I叮r下的分离
则几乎不受湿度影响，但其定量有差异，300ng点样量9％湿度下峰高为65％的
l．5倍左右。
温度对农药的分离影响不大，但对定量有影响，300ng／斑点4OC下所测得峰
高为 30C下的 1．01～l．23倍。
扫描狭缝的大小直接影响着定量，实验表明：物质最灵敏的扫描狭缝大小总
是小于其点样带宽的大小，并且狭缝的长度比宽度影响要大，当带宽为4与smm
时，样品展开后，用 2．00 X 0．20mm的狭缝扫描的峰高与峰面积均最大，6mm带宽
则用 4．00 X 0．30mm的狭缝最灵敏。
3．最小检测量和方法精密度。7种农药的最小检测限分别为西维因：Zng；味
哺丹、抗蚜威、灭多威、涣氰菊酯、甲氰菊酯与联苯菊酯均为 10ng；定量限分别
为4种氨基甲酸酯30ng，3种拟除虫菊酯20ng。50ng含量农药在上述展开方法
1展开后，无论是薄层扫描仪的精密度，还是包括点样精密度、簿层均匀度及展
开后有无边缘效应等的方法精密度，都是以峰高作为定量依据优于以峰面积作为
定量依据，对于上述7种农药，以峰高作为定量依据，薄层扫描仪检测相对标准
偏差（RSD）是在 1．07％－3．96％，方法 RSD在 3．61％－10．94％。
4．以马铃薯、冬瓜、青菜、空心菜、大豆和豆角等6种蔬菜为对象，分别建
立了4种氨基甲酸酯、3种拟除虫菊酯杀虫剂的HPTLC残留分析方法。实验表明：
由于蔬菜基质中杂质的影响，需对展开方法进行调整。
4种氨基甲酸酯杀虫剂的展开方法，Ic。r相应调整为在常温与大于 72％湿度
下上行展开，先用甲苯－丙酮（8：2，V八）展45VV，再用二氯甲烷－甲苯（：2，V灯）展
80mm，最后用二氯甲烷展到 80mm；11帕r被在 18％湿度下水平展开，先用二氯甲
烷－丙酮四：l，v／v）展 35mm，再用二氯甲烷展到 80mm代替。s种拟除?
In this paper, studies were conducted to determination the residues of pirimicarb, methomyl, carbaryl, carbofuran, fenpropathrin, deltamethrin and bifenthrin in vegetables with high-performance thin-layer chromatography(HPTLC). The factors that affected the determination were further investigated. The main results were summarized as following:
1. Two mobile phases were selected in two-trough chamber under normal temperature(4-20癈) and humidity (50-100%) for separating the pesticides standard. If mobile phase was toluene-acetone(7:3,v/v), the Rf valve of pirimicarb and methomyl were 0.66 and 0.37, while the Rf were 0.76 and 0.44 with petroleum ether-acetate ethyl(5:5,v/v). The first of carbofuran and carbaryl was dichloromethane-toluene-acetate ethyl(8:1:1,v/v) with the Rfof 0.48 and 0.63, and second was chloroform with the Rfof 0.25 and 0.50. The mobile phases of deltamethrine and fenpropathrin were toluene (0.77 and 0.63), and cyclohexane-chlorofornn (5:5,v/v) ( 0.47 and 0.40). Bifenthrin could be developed with toluene-petroleum ether (5:5,v/v) and cyclohexane-chloroform(8:2,v/v) respectively, the corresponding Rfwere 0.73 and 0.54 . All the mobile phases for single pesticides provide a theoretical base for mixed pesticides.
For 4 carbamates, the first system ( I car) was toluene-acetone(8:2,v/v) and dichloromethane-acetone(8:2,v/v). The migration distances were 45mm and 70mm respectively. Second one(IIcar) was petroleum ether- ethyl acetate (4:6,v/v) with 35mm, and then petroleum ether-chloroform (9:1,v/v) with 70mm.Toluene-petroleum ether(8:3,v/v) was system I pyr for 3 pyrethroids. And II pyr was cyclohexane -chloroform(5:5, v/v). The migration distances are both 70mm. Since the resolution (R) of pirimicarb and methomyl, carbofuran and carbaryl, fenpropathrin and deltamethrin, are 2.36,1.56,1.17 with mobile phase I car and I pyr, which are superior to that of II car and II pyr Especially separation of fenpropathrin and deltamethrin was not idea for 0.87 with II pyr So the former two were for quantification, the latter two were for qualification if they would work well in vegetables.
2. The factors that affected the determination:
When the speed of sample injection was within the range of 4s/ul to 15s/ul, the peak heights of contents of 20,50,100,200 and 300ng with 15s/ul were higher than that of 4s/ul by 2.9,2.6,1.5,1.3 and 1.1 times respectively. While the long time spent in the sample injection make the chances that thin-layer after activation absorbed vapour in air increased. 10s/ul was proper according to its time and effect.
The quantification and separation of pesticides were also affected by the band. For the contents of 20,50,100,200 and 300ng, the peak heights of them were194.2-382.9AU
with the band of 1mm , decreasing to106.3~326.3AU with that of 10mm. The separation of pirimicarb and methomyl was affected greatly by the band. R increased by 1.3 times when the band was from 3mm to 10mm. The band also affected the separation of 3 pyrethroids and impurity in spiked green vegetables. So 6mm was selected as the band width of sample injection.
Among the humidity of 9%, 14%, 18%, 32%, 42%, 47%, 65%, 72% and over 72%, 4 carbamates were separated best with mobile phase I Car in the humidity of over 72%, and the separation effect of 3 pyrethroids was not affected by humidity with I pyr, while the quantification was related to humidity. The peak heights of SOOng content of pyrethroids after development in the humidity of 9% were more than that in 65% by 1.5 times.
Studies also manifested that the peak heights of 300ng content after development in 4'C were 1.01 to 1.23 times as that in 30℃, while separation of 7 pesticides were good in both temperature.
The scanner slit was a main factor to determination. Results showed that the favourable scanner slit was always smaller than the band of sample injection, and the length was more important than the width of the scanner slit. When the band was 4mm or 5mm after development, the slit of 2.00×0.20mm was idea.
引文
1 韩熹莱主编．《农药概论》，北京农业大学出版社：1．
2 我国蔬菜产业持续发展面临难题．信息快递，蔬菜，2002，3：43．
3 裘孟荣．论提高茶叶的国际竞争力．茶叶，2002，28(1)：34，
4 岳永德，花日茂，张承祥主编．《茶叶农药残留与控制》．中国农业出版社：50—61．
5 吴锡端．2001年茶叶经济形势分析．中国茶叶，2002，24(1)．
6 中国农业百科全书，农药卷．农业出版社，北京．1993年10月：300，94．
7 刘忠．茶叶中多种拟除虫菊酯农药残留的测定．中国卫生检验杂志，2001，6：684．
8 Stefani R.,M. Buzzi, R.Grazzi. Supercritical fluid extraction of pesticide residues in fortified apple matrices.Journal of Chromatography A,1997,782:123-132.
9 汤锋，岳永德，花日茂，葛世玫，耿少芳．板兰根中多种拟除虫菊酯杀虫剂的残留分析．农药学学报，2001，1：69—72．
10 夏会龙．水中拟除虫菊酯类农药的分析．环境化学，1991，4：60。
11 Mastovska Katerina, Steven J. Lehotay,Jana Hajslova. Optimization and evaluation of low-pressure gas chromatography-mass spectrometry for the fast analysis of multiple pesticide residues in a food commodity. Journal of Chromatography A, 2001, 926:287-296.
12 Rossi S., A.P. Dalpero, S. Ghini, R. Colombo, A.G. Sabatini, S. Girotti. Multiresidual method for the gas chromatographic analysis of pesticides in honeybees cleaned by gel per permeation chromatography. Journal of Chromatography A,2001, 905:223-232.
13 Zrostlikova Jitka, Jana Hajslova, Michal Godula, Kaerina Mastovska. Performance of programmed temperature vaporizer pulse splitless and on-column injection techniques in analysis of pesticide residues in plant matrices. Journal of Chrom-atography A ,2001, 937:73-86.
14 Kocourek Vladimir,Jana Hajslova, Katerina Holadova, Jan Poustka.Stability of pesticides in plant extracts used as calibrants in the gas chromatographic analysis of residues. Journal of Chromatography A, 1998, 800:297-304.
15 Moffatt F., P.A. Cooper, K.M. Jessop. Comparison of capillary electrochromatograthy with high-performance liquid chromatography for the analysis of pirimicarb and related compounds.Journal of Chromatography A, 1999, 855:215-226.
16 Mijeong Lee Jeong, David J. Chesney. Determination of N-methylcarbamate pesticides from spiked matrices using supercritical fluid exraction. Analytica Chimica Acta, 1999, 389:53-57.
17 Carabias-MartineR, z,E. Rodriguez-Gonzalo, P.H. Paniagua-Marcos, J. Hernandez-Mendez.Analysis of pesticide residues in matrices with high lipid contents by membrane separation coupled on-line to a high-performance liquid chromatography system.
Journal of Chromatography A,2000,869:427-439.
18 张洪兰．用固相提取和高效液相色谱法分离检测生物体液中7种氨基甲酸酯农药．色谱，1997，15(5)：442-444．
19 段文仲，郝冬生．高效液相色谱法同时测定水果中多种农药残留量的方法的研究．农药，1998，8：20-22．
20 杨仁斌．氨基甲酸酯类农药的分析．环境化学，1995，3：288．
21 马志超，储可铭．液相色谱多残留测定氨基甲酸酯农药的方法．浙江农业大学学报，1995，21(4)：403-406．
22 Brain D.,Mc Garvey. High-performance liquid chromatographic methods for the determination of N-methyl carbamate pesticides in water, soil, plants and air.J.chromato.1993,642:89-105.
23 杨大进，张莹，方从容．大米中有机磷和氨基甲酸酯农药残留毛细管气相色谱测定法[J]．卫生研究，1994，23(2)：97-100．
24 谢恩平，林亲铁．克百威与丁硫克百威的残留与降解研究进展．农药科学与管理，2002，23：18-20．
25 Lacassie Eric,Pierre Marquet,Jean-Michel Galier, Marie-Framcoise Dreyfuss, Gerard Lachatre.Sensitive and specific multiresidue methods for the determination of pesticides of various classes in clinical and forensic toxicology. Forensic Science International,2001,121:116-125.
26 Lu Xuesong, Shane S.Que Hee. Permeation of methomyl in Lannate LTM through nitrile gloves.Journal of Hazardous Materials,1998,59:279-285.
27 Hardt Jochen,Uwe Appl,Jurgen Angerer.Biological monitoring of exposure to pirimicarb: hydroxypyrimidines in human urine.Toxicology Letters,1999,107:89-93.
28 Shinji Ito,Keiko Kudo, Tohru Imamura, Tsuneo Suzuki,Noriaki Ikeda.Sensitive determination of methomyl in blood using gas chromatography-mass spectrometry as its oxime tert.-butyldimethylsilyl derivative.Journal of Chromatography B,1998,713:323-330.
29 Salau J.S., M. Honing, R. Tauler,U. Barcelo. Resolution and quantitative determination of coeluted pesticide mixtures in liquid chromatography-thermospray mass spectrometry by multivariate curve resolution.Journal of Chromatography A, 1998,795:3-12.
30 Wan Chuanhao, Peter de B, Harrington. Screening GC-MS data for carbamate pesticides with temperature-constrained-cascade correlation neural networks. Analytica Chimica Acta,2000,408:1-12.
31 Hardt Jochen, Jurgen Angerer.Determination of metabolites of pirimicarb in human urine by gas chromatography-mass spectrometry.Journal of Chromatography B,
1999,730:229-238.
32 何丽一编著．平面色谱方法及应用．化学工业出版社：2．
33 Dubhashi S.S.,P.R Vavia.HPTLC method to study skin permeation of acylovir.Journal of Pharmaceutical and Biomedical Analysis, 2000,23:1017-1022.
34 岳永德．高效薄层析进行农药吸附态光解的研究．环境科学，1995，4：16—18．
35 王德利，唐福军，王朝清，肖翠红．薄层层析-紫外分光光度法测定玉米种衣剂有效成份含量研究．黑龙江八一农垦大学学报，1999，2：1-3．
36 Coran S.A., M. Bambagiotti-Alberti, V. Giannellini, A. Baldi,G. Picchioni, F. Paoli.Development of a densitometric method for the determination of cephalexin as an alternative to the standard HPLC procedure. Journal of Pharmacertical and Biological Analysis,1998,18:271-274.
37 李楠，覃柳琼，陈年春．薄层-紫外分光光度法分析辛-灭乳油中灭多威含量．农药，1997，36(2)：24-25．
38 Howard A.G.,T. Shafik, F.Moffatt,I.D. Wilson. Electroosmotically driven thin-layer electrochromatography on silica media. Journal of Chromatography A, 1999,844:333-340
39 Lautie J.P.,V. Stankovic, G. Sinoquet. Determination of chlormequat in pears by high-performance thin layer chromatography and high-performance liquid chromatography with conductimetric detedtion. Analysis, 2000, 28: 155-158.
40 Mohammad, A.,Anwar, S.,Iraqi, Eram, TLC in organic environmental analysis.J. Chem. Environ, 1998,2(1).
41 Milhail K, Beklemishev, Alexey L, Kapanadze, Natalya V. Bakhilina, Inga F. Dolmanova. Accelerating effect of silica on the indicator reaction o-dianisidine-H_2O_2. Talanta,2000,51:389-394.
42 Rathore. H.S., Begun, T. Thin-layer chromatographic methods for use in pesticide Analysis.J. Chromatogr., 1993,643: 271-290.
43 Sherma. J. Determination of pesticides by thin-layer chromatography. J Planner Chromatogr.,1994,7:265-272.
44 Coran S.A., M. Bambagiotti-Alberti, V. Giannellini, A. Baldi, G. Picchioni. Development of a densitometric method for the determination of cephalexin as an alternative to the standard HPLC procedure.Journal of Pharmaceutical and Biomedical Analysis, 1998,18:271-274.
45 Niewiadomy Andrzej, Anna Zabinska, Joanna Matysiak, Jan K. Rozy. Influence of modifier and molecular structure of somedihydroxythiobenzanilides on retention in reversed-phase high-performance thin-layer chromatography. Journal of Chromatography A, 1997,791,237-243.
46 De Leenheer A P et al.Modern Chromatographic Analysis of the Vitamins. New York:
Marcel Dekker, 1985:216.
47 林乐明，张军，黄胜起．应用一维薄层色谱法测定羊水磷脂化合物预测胎儿成熟度．色谱，1994，12：171．
48 常理文，郭京力，余君．血清中微量神经节苷脂的色谱分析．色谱，1994，12：189．
49 Nabi,S.A.,Islam,.Ranman, N. Acta Chromatogr.,2000,10:213-221.
50 Camag Bibliography Service (CBS),2000, 85:7.
51 Butz S., H. J. Stan. Screening of 265 Pesticides in Water by Thin-Layer Chromatography with Automated Multiple Development.Analytical Chemistry, 1995,67(3):620-630.
52 Das, S.,Moharana, S.N.,Patel, S.N..Teach. Res. Chem.,1998,5:15-17.
53 Kapanadze, A.L.,Beklemishev, M.K.,Dolmanova.I.F,,J. Anal. Chem.,1999,54:1047-1052.
54 Gupta, S.,Handa, S.K., Sharma, K.K..A new spay reagent for the detection of synthetic pyrethroids containing a nitrile group on thin-layer plates.Talanta, 1998,45:1111-1114.
55 Rathore, Hamir Singh, Mital, Sheetal. Spot test analysis of pesticides:TLC detection of mancozeb. Mod. TLC, 1997,10(2):124-127.
56 Ohnishi-Kameyama, Mayumi, Nagata, Tadahiro. An application of x-ray fluorescence spectrometry to the study of thin-layer chromatography.Anal Chem,1998,70(9):1916-1920.
57 Sherma Josep. Recent Advances in Thin-Layer Chromatography of Pestides. AOAC International, 2001, 84(4).
58 Babic, S., Petrovic, M.,Kastelan-Macan, M.. Ultrasonic solvent extraction of pesticides from soil. J. Chromatogr. A, 1998,823:3-9.
59 ladek, J,;Rostkowski, A,, Miszczak, M..Application of instrumental thin- layer chromatography and solid-phase extraction to the analyses of pesticide residues in grossly contaminated samples of soil.J.Chromatogr.,A,1996,754(1+2):273-278.
60 Sun, B.Chinese J. Chromatogr.1999, 17:93-94.
61 Rane, K.D., Mall, B.D., Garad, M.V., Patil, V.B., J. PlanarChromatogr.-Mod.TLC, 1998, 11:74-76.
62 Futagami Koujiro,Chie Narazaki,Yasufumi Kataoka,Hideki Shuto,Ryozo Oishi. Application of high-performance thin-layer chromatography for the detection of organophosphorus insecticides in human serum after acute poisoning.Journal of Chromatography B,1997,704:53-58.
63 Funk Werner,Luise Cleres,Hoiger Pitzer,Gerhild Donnevert.Organophosphorus insecticides-quantitative HPTLC determination and characterization.Journal of Planner Chromatography.1989,641:285-288.
64 Rawat, J.P.,Bhardwaj, M..Thin layer chromatographic behavoir of organophosphate pesticides on hydrated stannic oxide layers.Orient.J. Chem, 2000,16(1):53-58.
65 Yao, Hongbin. Pesticide residues in fruits at market. Nongyao Kexue Yu Guanli,1998,19:9-10.
66 吕桂芸，骆天祜．薄层层析-溴化法测定水胺硫磷，农药，1995，Vol．34，No．4：29-31．
67 Kempe, G.,Schumann. U.. Speer. K., Dtsch., 1999.
68 Rane, g.D.,Mali, B.D.,Garad, M.V..J. Planar Chromatogr.-Mod. TLC, 1997,10:89-91.
69 Sharma, A.K., Sharma, J.D..J. Environ. Biol.,1999, 20:89-91.
70 钱传范主编．农药分析．北京农业大学：20．
71 Patil V.B, Shingare M S..J Planar Chromagr.,1995, 8:160.
72 Babic, S., Petrovic, M., Kastelan-Macan, M.. Optimization of chromatographic separation of pesticides. Kem. Ind, 1998,47(7-8):275-279.
73 Petrovic, Mira, Kastelan-Macan, Marija, Babic, Sandra. Qrantitative evaluation of 2D chromatograms with a CCD camera. J. Planaar Chromatogr.-Mod TLC, 1998,11(5):353-356.
74 Tomasz Tuzimski, Edward Soczewinski. Correlation parameters of pesticides in normal-and reversed-phase systems and their utilization for the separation of a mixture of 14 triazines and urea herbicides by means of two-dimensional thin-layer chromatography.Journal of Chromatography A. 2002, 961:277-283.
75 Hans-Jurgen Stan, Fred Schwarzer. On-line coupling of liquid chromatography with thin-layer chromatography.Journal of Chromatography A. 1998,819:35-44.
76 Gupta, S.,Sharma, K.K.,Handa, S.K..Fourier transform infrared spectroscopic determination of cypermethrin and deltamethrin emulsifiable conentrate formations. Talanta, 1997,44:2075-2079.
77 Sang-Ki Lee, Kiyoshi Ameno, Sang-Whan In, Won-Kyung Yang, Ki-seo Koo, Young-Chan Yoo, Takako Kubota, Setsuko Ameno,Iwao Ijiri. Acute fatal poisoning cases due to furathiocarb ingestion. Forensic Science International, 1999,101:65-70.
78 Kiyoshi Ameno, Sang-Ki Lee, Sang-Whan In, Ja-Yeol Yang, Young-CMn Yoo, Setsuko Ameno,Takako Kubota, Hiroshi Kinoshita,Iwao Ijiri. Blood carbofuran concentrations in suicidal ingestion cases.Forensic Science International, 2001,116:59-61.
79 Elsirafy A.A., A.A. Ghanem, A.E. Eid, S.A. Eldakroory. Chronological study of diazinon in putrefied viscera of rats using GC/MS, GC/EC and TLC. Forensic Science International,2000,109:147-157.
80 Sherma Josep. Planar Chromatography, Analytical Chemidtry, 1998, 70(12):7-26.
81 闻培武编译．农药薄层色谱分析法的最新进展．世界农药(原《农药译丛》)，1999，21(5)：44-45．
82 Sherma Josep. Thin-layer chromatography in food and agricultural analysis. Journal
of chromatography A, 2000,880:129-147.
83 Sherma J.. Thin Layer Chromatography in Environmental Analysis. Reviews in Analytical Chemistry, 1995,2:75-124.
84 Sherma J.. Thin Layer Chromatography in Food Analysis. Food Testing and Analysis,1996,2(2):39-44.
85 刘玉萍，张明娜．入世后我国蔬菜产业面临的形势及对策。中国蔬菜，2002(1)：1-3．
86 张德纯，刘肃，钱洪．浅析我国蔬菜产品安全质量标准．中国农业科技导报，2002，4(5)．
87 何玲芳，财俊良．怎样消除蔬菜上的残留农药．蔬菜，2002(3)：23．
88 李治祥．关于安徽省农药残留与农产品质量检测体系建设的探讨．农药科学与管理，2002，23(5)：29-30．
89 郭立，张清明．氨基甲酸酯类农药残留分析方法进展．天津农学院学报，2001，8(4)：15-21．
90 Nunes G.S., M.L. Ribeiro, L. Polese, D. Barcelo. Comparsion of different clean-up produres for the determination of N-methylcarbamate insectides in vegetable matrices by high-performance liquid chromagraphy with UV detection. Journal of Chromatography A,1998,795:43-51.
91 Antonio Abad, Maria Jose Moreno, Rosa Pelegri, Maria Isabel Martinez, Adolfo Saez,Miguel Gamon, Angel Montoya. Determiation of carbaryl, carbofuran and methiocarb in cucumbers and strawberries by monoclonal enzyme immunoassays and high-performance liquid chromatography with fouorescence detection An analytical comparison, Journal of Chromatography A, 1999,833:3-12.
92 李萍．氨基甲酸酯农药残留分析方法[J]．国外医学卫生学分册，1999，26(6)：366-370．
93 Santos Delgado M.J.,S. Rubio Barriso, G. Toledano Fernandez-Tostado, L.M. Polo-Diez.Stability studies of carbamate pesticides and analysis by gas chromatography with flame ionisation and nitrogen-phosphorus detection.Journal of Chromatography A, 2000, 921:287-296.
94 杨大进，方从容，张莹．蔬菜中有机磷和氨基甲酸酯农药残留测定[J]．中国食品卫生杂志，1992，9(5)：9-11．
95 Nunes M.S.,D.Barcelo, B.S. Gr.abaric,J.M.Diaz-Cruz, M.L. Ribeiro. Evaluation of a highly sensitive amperometric biosensor with low cholinesterase charge immobiliz on a chemically modified carbon paste electrode for trace determinationed of carbamates in fruit, vegetable and water samples. Analytica Chimica Acta, 1999,399:37-49.
96 王筠．拟除虫菊酯综述．安徽化工，1997，4：5-7．
97 张夏亭．天然除虫菊的开发及应用．农药科学与管理，2002，23(2)：25．
98 Altenkirch, H., Hopmann, D., Brockmeier, B., Walter, G.. Neurological investigations in 23 cases of pyrethroid intoxication reported to the General Federal Health
Office..Neurotoxicology,1996,17:645-651.
99 Colume A.,S. Cardenas, M. Gallego, M. Valcarcel. Semiartomatic multiresidue gas chromatographic method for the screening of vegetables for 25 organochlurine and pyrethroid pesticides. Analytica Chimica Acta, 2001, 436:153-162.
100 Motohashi Boru, Hideo Nagashima, Cyril Parkanyi. Supercritical fluid extraction for the analysis of pesticide residues in miscellaneous samples. J. Bilchem. Biophys.Methods, 2000,43:313-328.
101 华南农业大学主编．植物化学保护(第二版)．农业出版社：152-153，170，175．
102 农药管理与使用标准汇编．中国标准出版社，2002：34，38，51．
103 中国出版社第一编辑室编．中国食品工业标准汇编水果蔬菜及其制品卷．中国标准出版社，1999：38．
104 中国人民共和国农业部农药检定所编．农产品农药残留限量标准汇编．中国农业出版社．
2 我国蔬菜产业持续发展面临难题．信息快递，蔬菜，2002，3：43．
3 裘孟荣．论提高茶叶的国际竞争力．茶叶，2002，28(1)：34，
4 岳永德，花日茂，张承祥主编．《茶叶农药残留与控制》．中国农业出版社：50—61．
5 吴锡端．2001年茶叶经济形势分析．中国茶叶，2002，24(1)．
6 中国农业百科全书，农药卷．农业出版社，北京．1993年10月：300，94．
7 刘忠．茶叶中多种拟除虫菊酯农药残留的测定．中国卫生检验杂志，2001，6：684．
8 Stefani R.,M. Buzzi, R.Grazzi. Supercritical fluid extraction of pesticide residues in fortified apple matrices.Journal of Chromatography A,1997,782:123-132.
9 汤锋，岳永德，花日茂，葛世玫，耿少芳．板兰根中多种拟除虫菊酯杀虫剂的残留分析．农药学学报，2001，1：69—72．
10 夏会龙．水中拟除虫菊酯类农药的分析．环境化学，1991，4：60。
11 Mastovska Katerina, Steven J. Lehotay,Jana Hajslova. Optimization and evaluation of low-pressure gas chromatography-mass spectrometry for the fast analysis of multiple pesticide residues in a food commodity. Journal of Chromatography A, 2001, 926:287-296.
12 Rossi S., A.P. Dalpero, S. Ghini, R. Colombo, A.G. Sabatini, S. Girotti. Multiresidual method for the gas chromatographic analysis of pesticides in honeybees cleaned by gel per permeation chromatography. Journal of Chromatography A,2001, 905:223-232.
13 Zrostlikova Jitka, Jana Hajslova, Michal Godula, Kaerina Mastovska. Performance of programmed temperature vaporizer pulse splitless and on-column injection techniques in analysis of pesticide residues in plant matrices. Journal of Chrom-atography A ,2001, 937:73-86.
14 Kocourek Vladimir,Jana Hajslova, Katerina Holadova, Jan Poustka.Stability of pesticides in plant extracts used as calibrants in the gas chromatographic analysis of residues. Journal of Chromatography A, 1998, 800:297-304.
15 Moffatt F., P.A. Cooper, K.M. Jessop. Comparison of capillary electrochromatograthy with high-performance liquid chromatography for the analysis of pirimicarb and related compounds.Journal of Chromatography A, 1999, 855:215-226.
16 Mijeong Lee Jeong, David J. Chesney. Determination of N-methylcarbamate pesticides from spiked matrices using supercritical fluid exraction. Analytica Chimica Acta, 1999, 389:53-57.
17 Carabias-MartineR, z,E. Rodriguez-Gonzalo, P.H. Paniagua-Marcos, J. Hernandez-Mendez.Analysis of pesticide residues in matrices with high lipid contents by membrane separation coupled on-line to a high-performance liquid chromatography system.
Journal of Chromatography A,2000,869:427-439.
18 张洪兰．用固相提取和高效液相色谱法分离检测生物体液中7种氨基甲酸酯农药．色谱，1997，15(5)：442-444．
19 段文仲，郝冬生．高效液相色谱法同时测定水果中多种农药残留量的方法的研究．农药，1998，8：20-22．
20 杨仁斌．氨基甲酸酯类农药的分析．环境化学，1995，3：288．
21 马志超，储可铭．液相色谱多残留测定氨基甲酸酯农药的方法．浙江农业大学学报，1995，21(4)：403-406．
22 Brain D.,Mc Garvey. High-performance liquid chromatographic methods for the determination of N-methyl carbamate pesticides in water, soil, plants and air.J.chromato.1993,642:89-105.
23 杨大进，张莹，方从容．大米中有机磷和氨基甲酸酯农药残留毛细管气相色谱测定法[J]．卫生研究，1994，23(2)：97-100．
24 谢恩平，林亲铁．克百威与丁硫克百威的残留与降解研究进展．农药科学与管理，2002，23：18-20．
25 Lacassie Eric,Pierre Marquet,Jean-Michel Galier, Marie-Framcoise Dreyfuss, Gerard Lachatre.Sensitive and specific multiresidue methods for the determination of pesticides of various classes in clinical and forensic toxicology. Forensic Science International,2001,121:116-125.
26 Lu Xuesong, Shane S.Que Hee. Permeation of methomyl in Lannate LTM through nitrile gloves.Journal of Hazardous Materials,1998,59:279-285.
27 Hardt Jochen,Uwe Appl,Jurgen Angerer.Biological monitoring of exposure to pirimicarb: hydroxypyrimidines in human urine.Toxicology Letters,1999,107:89-93.
28 Shinji Ito,Keiko Kudo, Tohru Imamura, Tsuneo Suzuki,Noriaki Ikeda.Sensitive determination of methomyl in blood using gas chromatography-mass spectrometry as its oxime tert.-butyldimethylsilyl derivative.Journal of Chromatography B,1998,713:323-330.
29 Salau J.S., M. Honing, R. Tauler,U. Barcelo. Resolution and quantitative determination of coeluted pesticide mixtures in liquid chromatography-thermospray mass spectrometry by multivariate curve resolution.Journal of Chromatography A, 1998,795:3-12.
30 Wan Chuanhao, Peter de B, Harrington. Screening GC-MS data for carbamate pesticides with temperature-constrained-cascade correlation neural networks. Analytica Chimica Acta,2000,408:1-12.
31 Hardt Jochen, Jurgen Angerer.Determination of metabolites of pirimicarb in human urine by gas chromatography-mass spectrometry.Journal of Chromatography B,
1999,730:229-238.
32 何丽一编著．平面色谱方法及应用．化学工业出版社：2．
33 Dubhashi S.S.,P.R Vavia.HPTLC method to study skin permeation of acylovir.Journal of Pharmaceutical and Biomedical Analysis, 2000,23:1017-1022.
34 岳永德．高效薄层析进行农药吸附态光解的研究．环境科学，1995，4：16—18．
35 王德利，唐福军，王朝清，肖翠红．薄层层析-紫外分光光度法测定玉米种衣剂有效成份含量研究．黑龙江八一农垦大学学报，1999，2：1-3．
36 Coran S.A., M. Bambagiotti-Alberti, V. Giannellini, A. Baldi,G. Picchioni, F. Paoli.Development of a densitometric method for the determination of cephalexin as an alternative to the standard HPLC procedure. Journal of Pharmacertical and Biological Analysis,1998,18:271-274.
37 李楠，覃柳琼，陈年春．薄层-紫外分光光度法分析辛-灭乳油中灭多威含量．农药，1997，36(2)：24-25．
38 Howard A.G.,T. Shafik, F.Moffatt,I.D. Wilson. Electroosmotically driven thin-layer electrochromatography on silica media. Journal of Chromatography A, 1999,844:333-340
39 Lautie J.P.,V. Stankovic, G. Sinoquet. Determination of chlormequat in pears by high-performance thin layer chromatography and high-performance liquid chromatography with conductimetric detedtion. Analysis, 2000, 28: 155-158.
40 Mohammad, A.,Anwar, S.,Iraqi, Eram, TLC in organic environmental analysis.J. Chem. Environ, 1998,2(1).
41 Milhail K, Beklemishev, Alexey L, Kapanadze, Natalya V. Bakhilina, Inga F. Dolmanova. Accelerating effect of silica on the indicator reaction o-dianisidine-H_2O_2. Talanta,2000,51:389-394.
42 Rathore. H.S., Begun, T. Thin-layer chromatographic methods for use in pesticide Analysis.J. Chromatogr., 1993,643: 271-290.
43 Sherma. J. Determination of pesticides by thin-layer chromatography. J Planner Chromatogr.,1994,7:265-272.
44 Coran S.A., M. Bambagiotti-Alberti, V. Giannellini, A. Baldi, G. Picchioni. Development of a densitometric method for the determination of cephalexin as an alternative to the standard HPLC procedure.Journal of Pharmaceutical and Biomedical Analysis, 1998,18:271-274.
45 Niewiadomy Andrzej, Anna Zabinska, Joanna Matysiak, Jan K. Rozy. Influence of modifier and molecular structure of somedihydroxythiobenzanilides on retention in reversed-phase high-performance thin-layer chromatography. Journal of Chromatography A, 1997,791,237-243.
46 De Leenheer A P et al.Modern Chromatographic Analysis of the Vitamins. New York:
Marcel Dekker, 1985:216.
47 林乐明，张军，黄胜起．应用一维薄层色谱法测定羊水磷脂化合物预测胎儿成熟度．色谱，1994，12：171．
48 常理文，郭京力，余君．血清中微量神经节苷脂的色谱分析．色谱，1994，12：189．
49 Nabi,S.A.,Islam,.Ranman, N. Acta Chromatogr.,2000,10:213-221.
50 Camag Bibliography Service (CBS),2000, 85:7.
51 Butz S., H. J. Stan. Screening of 265 Pesticides in Water by Thin-Layer Chromatography with Automated Multiple Development.Analytical Chemistry, 1995,67(3):620-630.
52 Das, S.,Moharana, S.N.,Patel, S.N..Teach. Res. Chem.,1998,5:15-17.
53 Kapanadze, A.L.,Beklemishev, M.K.,Dolmanova.I.F,,J. Anal. Chem.,1999,54:1047-1052.
54 Gupta, S.,Handa, S.K., Sharma, K.K..A new spay reagent for the detection of synthetic pyrethroids containing a nitrile group on thin-layer plates.Talanta, 1998,45:1111-1114.
55 Rathore, Hamir Singh, Mital, Sheetal. Spot test analysis of pesticides:TLC detection of mancozeb. Mod. TLC, 1997,10(2):124-127.
56 Ohnishi-Kameyama, Mayumi, Nagata, Tadahiro. An application of x-ray fluorescence spectrometry to the study of thin-layer chromatography.Anal Chem,1998,70(9):1916-1920.
57 Sherma Josep. Recent Advances in Thin-Layer Chromatography of Pestides. AOAC International, 2001, 84(4).
58 Babic, S., Petrovic, M.,Kastelan-Macan, M.. Ultrasonic solvent extraction of pesticides from soil. J. Chromatogr. A, 1998,823:3-9.
59 ladek, J,;Rostkowski, A,, Miszczak, M..Application of instrumental thin- layer chromatography and solid-phase extraction to the analyses of pesticide residues in grossly contaminated samples of soil.J.Chromatogr.,A,1996,754(1+2):273-278.
60 Sun, B.Chinese J. Chromatogr.1999, 17:93-94.
61 Rane, K.D., Mall, B.D., Garad, M.V., Patil, V.B., J. PlanarChromatogr.-Mod.TLC, 1998, 11:74-76.
62 Futagami Koujiro,Chie Narazaki,Yasufumi Kataoka,Hideki Shuto,Ryozo Oishi. Application of high-performance thin-layer chromatography for the detection of organophosphorus insecticides in human serum after acute poisoning.Journal of Chromatography B,1997,704:53-58.
63 Funk Werner,Luise Cleres,Hoiger Pitzer,Gerhild Donnevert.Organophosphorus insecticides-quantitative HPTLC determination and characterization.Journal of Planner Chromatography.1989,641:285-288.
64 Rawat, J.P.,Bhardwaj, M..Thin layer chromatographic behavoir of organophosphate pesticides on hydrated stannic oxide layers.Orient.J. Chem, 2000,16(1):53-58.
65 Yao, Hongbin. Pesticide residues in fruits at market. Nongyao Kexue Yu Guanli,1998,19:9-10.
66 吕桂芸，骆天祜．薄层层析-溴化法测定水胺硫磷，农药，1995，Vol．34，No．4：29-31．
67 Kempe, G.,Schumann. U.. Speer. K., Dtsch., 1999.
68 Rane, g.D.,Mali, B.D.,Garad, M.V..J. Planar Chromatogr.-Mod. TLC, 1997,10:89-91.
69 Sharma, A.K., Sharma, J.D..J. Environ. Biol.,1999, 20:89-91.
70 钱传范主编．农药分析．北京农业大学：20．
71 Patil V.B, Shingare M S..J Planar Chromagr.,1995, 8:160.
72 Babic, S., Petrovic, M., Kastelan-Macan, M.. Optimization of chromatographic separation of pesticides. Kem. Ind, 1998,47(7-8):275-279.
73 Petrovic, Mira, Kastelan-Macan, Marija, Babic, Sandra. Qrantitative evaluation of 2D chromatograms with a CCD camera. J. Planaar Chromatogr.-Mod TLC, 1998,11(5):353-356.
74 Tomasz Tuzimski, Edward Soczewinski. Correlation parameters of pesticides in normal-and reversed-phase systems and their utilization for the separation of a mixture of 14 triazines and urea herbicides by means of two-dimensional thin-layer chromatography.Journal of Chromatography A. 2002, 961:277-283.
75 Hans-Jurgen Stan, Fred Schwarzer. On-line coupling of liquid chromatography with thin-layer chromatography.Journal of Chromatography A. 1998,819:35-44.
76 Gupta, S.,Sharma, K.K.,Handa, S.K..Fourier transform infrared spectroscopic determination of cypermethrin and deltamethrin emulsifiable conentrate formations. Talanta, 1997,44:2075-2079.
77 Sang-Ki Lee, Kiyoshi Ameno, Sang-Whan In, Won-Kyung Yang, Ki-seo Koo, Young-Chan Yoo, Takako Kubota, Setsuko Ameno,Iwao Ijiri. Acute fatal poisoning cases due to furathiocarb ingestion. Forensic Science International, 1999,101:65-70.
78 Kiyoshi Ameno, Sang-Ki Lee, Sang-Whan In, Ja-Yeol Yang, Young-CMn Yoo, Setsuko Ameno,Takako Kubota, Hiroshi Kinoshita,Iwao Ijiri. Blood carbofuran concentrations in suicidal ingestion cases.Forensic Science International, 2001,116:59-61.
79 Elsirafy A.A., A.A. Ghanem, A.E. Eid, S.A. Eldakroory. Chronological study of diazinon in putrefied viscera of rats using GC/MS, GC/EC and TLC. Forensic Science International,2000,109:147-157.
80 Sherma Josep. Planar Chromatography, Analytical Chemidtry, 1998, 70(12):7-26.
81 闻培武编译．农药薄层色谱分析法的最新进展．世界农药(原《农药译丛》)，1999，21(5)：44-45．
82 Sherma Josep. Thin-layer chromatography in food and agricultural analysis. Journal
of chromatography A, 2000,880:129-147.
83 Sherma J.. Thin Layer Chromatography in Environmental Analysis. Reviews in Analytical Chemistry, 1995,2:75-124.
84 Sherma J.. Thin Layer Chromatography in Food Analysis. Food Testing and Analysis,1996,2(2):39-44.
85 刘玉萍，张明娜．入世后我国蔬菜产业面临的形势及对策。中国蔬菜，2002(1)：1-3．
86 张德纯，刘肃，钱洪．浅析我国蔬菜产品安全质量标准．中国农业科技导报，2002，4(5)．
87 何玲芳，财俊良．怎样消除蔬菜上的残留农药．蔬菜，2002(3)：23．
88 李治祥．关于安徽省农药残留与农产品质量检测体系建设的探讨．农药科学与管理，2002，23(5)：29-30．
89 郭立，张清明．氨基甲酸酯类农药残留分析方法进展．天津农学院学报，2001，8(4)：15-21．
90 Nunes G.S., M.L. Ribeiro, L. Polese, D. Barcelo. Comparsion of different clean-up produres for the determination of N-methylcarbamate insectides in vegetable matrices by high-performance liquid chromagraphy with UV detection. Journal of Chromatography A,1998,795:43-51.
91 Antonio Abad, Maria Jose Moreno, Rosa Pelegri, Maria Isabel Martinez, Adolfo Saez,Miguel Gamon, Angel Montoya. Determiation of carbaryl, carbofuran and methiocarb in cucumbers and strawberries by monoclonal enzyme immunoassays and high-performance liquid chromatography with fouorescence detection An analytical comparison, Journal of Chromatography A, 1999,833:3-12.
92 李萍．氨基甲酸酯农药残留分析方法[J]．国外医学卫生学分册，1999，26(6)：366-370．
93 Santos Delgado M.J.,S. Rubio Barriso, G. Toledano Fernandez-Tostado, L.M. Polo-Diez.Stability studies of carbamate pesticides and analysis by gas chromatography with flame ionisation and nitrogen-phosphorus detection.Journal of Chromatography A, 2000, 921:287-296.
94 杨大进，方从容，张莹．蔬菜中有机磷和氨基甲酸酯农药残留测定[J]．中国食品卫生杂志，1992，9(5)：9-11．
95 Nunes M.S.,D.Barcelo, B.S. Gr.abaric,J.M.Diaz-Cruz, M.L. Ribeiro. Evaluation of a highly sensitive amperometric biosensor with low cholinesterase charge immobiliz on a chemically modified carbon paste electrode for trace determinationed of carbamates in fruit, vegetable and water samples. Analytica Chimica Acta, 1999,399:37-49.
96 王筠．拟除虫菊酯综述．安徽化工，1997，4：5-7．
97 张夏亭．天然除虫菊的开发及应用．农药科学与管理，2002，23(2)：25．
98 Altenkirch, H., Hopmann, D., Brockmeier, B., Walter, G.. Neurological investigations in 23 cases of pyrethroid intoxication reported to the General Federal Health
Office..Neurotoxicology,1996,17:645-651.
99 Colume A.,S. Cardenas, M. Gallego, M. Valcarcel. Semiartomatic multiresidue gas chromatographic method for the screening of vegetables for 25 organochlurine and pyrethroid pesticides. Analytica Chimica Acta, 2001, 436:153-162.
100 Motohashi Boru, Hideo Nagashima, Cyril Parkanyi. Supercritical fluid extraction for the analysis of pesticide residues in miscellaneous samples. J. Bilchem. Biophys.Methods, 2000,43:313-328.
101 华南农业大学主编．植物化学保护(第二版)．农业出版社：152-153，170，175．
102 农药管理与使用标准汇编．中国标准出版社，2002：34，38，51．
103 中国出版社第一编辑室编．中国食品工业标准汇编水果蔬菜及其制品卷．中国标准出版社，1999：38．
104 中国人民共和国农业部农药检定所编．农产品农药残留限量标准汇编．中国农业出版社．