黔产主要中成药中农药残留的调查研究
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摘要
中成药农药残留问题是中成药现代化、国际化急待解决的问题之一。本研究是顺应贵州省中药现代化发展需要,对贵州省主要中成药的农药残留状况开展调查研究,并建立相应的检测方法。在此基础上,构建贵州省中成药农药残留检测平台,为实现中成药现代化、国际化提供技术支持,主要研究内容如下:
1收集了贵州省不同厂家生产的主要中成药,对其有机氯农药残留量进行测定,在71个中成药样品中,有52个检出有机氯农药,检出率73.24%,大部分样品的农药残留量均在0.01mg/kg以下。以《2005版药典》有机氯农药残留的限量标准为参照,没有农药超标;参照《药用植物及制剂进出口绿色行业标准》,超标率为1.4%。
2收集了贵州省不同厂家生产的主要中成药,对其拟除虫菊酯类农药残留量进行测定。建立了电子捕获检测器-毛细管气相色谱法测定中成药中拟除虫菊酯类农药残留的方法。样品平均回收率78.69%～113.52%。线性范围为:0.10～5.0μg/mL。适用于中成药中拟除虫菊酯类农药残留的测定。在71个中成药样品中,有25个检出菊酯类农药,检出率35.21%。以《欧盟茶叶中农药最大残留限量表》中拟除虫菊酯类农药残留的限量标准为参照,71个中成药样品没有农药超标。
3收集了贵州省不同厂家生产的主要中成药,对其有机磷农药残留量进行测定。建立了OV-1701毛细管柱-脉冲火焰光度检测器(PFPD)、气相色谱法测定中成药中有机磷农药残留量。所测定样品均未检出有机磷农药残留。这可能与有机磷农药降解周期相对较短,性质不稳定有关,中成药中一般不含有机磷类农药。
4建立以凝胶渗透色谱(GPC)净化,气相色谱法测定中成药中有机氯农药残留的方法。样品经丙酮,二氯甲烷提取,GPC净化,电子捕获检测器(ECD)检测。样品平均回收率:87.21%～109.54%,检出限范围:0.000182～0.003295μg/mL。适用于中成药的有机氯农药的检测。
The pesticide residue of Chinese traditional patent medicine is one of the problem that we need to be resolved when it is face of internationalization and modernization. This study is response to development needs of Modernization of Traditional Chinese Medicine of Guizhou Province, the corresponding detection methods were built by investigation on the pesticide residue of Chinese traditional patent medicine in Guizhou province. On this basis, a detection Platform of pesticide residues of Chinese traditional patent medicine in Guizhou Province was built to give the quality assurance and technical support for modern and international Chinese traditional patent medicine in Guizhou. Main content of the study are as follows :
1 The organochlorine pesticides residues were determined which from different major Chinese traditional patent medicine of Guizhou Province. The results showed that there have detected 52 organochlorine pesticides of 71 sample, and the detection rate of 73. 24%, the majority of samples pesticide residues is less than 0. Olmg/kg. According to Chinese Pharmacopoeia(2005 version) organochlorine pesticide residues of the limited standards, there is no excessive samples; referencing to "Green Trade Standards of Importing & Exporting Medicinal plants & Preparations" , over standard rate is 1.4%.
2 The Pyrethriods Pesticide residues were determined which from different major Chinese traditional patent medicine of Guizhou Province. To establish a method for determination Pyrethriods Pesticide in Chinese traditional patent medicine by the electron capture detector-capillary gas chromatography. The recoveries and RSD of Pyrethriods Pesticide were 78. 69%～113. 52%. The linear ranges were 0.10～5.0μg/mL It can be used to detect Pyrethriods Pesticide from Chinese traditional patent medicine. There were 25 of 71 sample was detected Pyrethriods Pesticide, and the detection rate is 35.21%. Referencing to "maximum residue limits of Tea in the European" , 71 samples of Chinese patent medicine did not exceed the standard.
3 The Organophosphorous Pesticide residues were determined which from different major Chinese traditional patent medicine of Guizhou Province. To establish a method for determination Organophosphorous Pesticide in Chinese traditional patent medicine by the pulsed flame photometric detector (PFPD)- gas chromatography, and the column was OV-1701 capillary column. all the samples were not detected of organophosphorus pesticide residues. This may be related to degradation period of organophosphorus pesticide is relatively short, the properties instability. Generally speaking, Chinese traditional patent medicine did not have organophosphorus pesticide.
4 To establish a method for determination Organochlorine pesticides in Chinese traditional patent medicine by -gas chromatography. The sample was extract with acetone , dichloromethane , GPC purification, and detected with electron capture detector (ECD). The recoveries of Organochlorine pesticides were 87. 21%～109. 54%. The detected limited were 0. 000182～0. 003295μg/mL. It can be used to detect Organochlorine pesticides from Chinese traditional patent medicine.
1收集了贵州省不同厂家生产的主要中成药,对其有机氯农药残留量进行测定,在71个中成药样品中,有52个检出有机氯农药,检出率73.24%,大部分样品的农药残留量均在0.01mg/kg以下。以《2005版药典》有机氯农药残留的限量标准为参照,没有农药超标;参照《药用植物及制剂进出口绿色行业标准》,超标率为1.4%。
2收集了贵州省不同厂家生产的主要中成药,对其拟除虫菊酯类农药残留量进行测定。建立了电子捕获检测器-毛细管气相色谱法测定中成药中拟除虫菊酯类农药残留的方法。样品平均回收率78.69%～113.52%。线性范围为:0.10～5.0μg/mL。适用于中成药中拟除虫菊酯类农药残留的测定。在71个中成药样品中,有25个检出菊酯类农药,检出率35.21%。以《欧盟茶叶中农药最大残留限量表》中拟除虫菊酯类农药残留的限量标准为参照,71个中成药样品没有农药超标。
3收集了贵州省不同厂家生产的主要中成药,对其有机磷农药残留量进行测定。建立了OV-1701毛细管柱-脉冲火焰光度检测器(PFPD)、气相色谱法测定中成药中有机磷农药残留量。所测定样品均未检出有机磷农药残留。这可能与有机磷农药降解周期相对较短,性质不稳定有关,中成药中一般不含有机磷类农药。
4建立以凝胶渗透色谱(GPC)净化,气相色谱法测定中成药中有机氯农药残留的方法。样品经丙酮,二氯甲烷提取,GPC净化,电子捕获检测器(ECD)检测。样品平均回收率:87.21%～109.54%,检出限范围:0.000182～0.003295μg/mL。适用于中成药的有机氯农药的检测。
The pesticide residue of Chinese traditional patent medicine is one of the problem that we need to be resolved when it is face of internationalization and modernization. This study is response to development needs of Modernization of Traditional Chinese Medicine of Guizhou Province, the corresponding detection methods were built by investigation on the pesticide residue of Chinese traditional patent medicine in Guizhou province. On this basis, a detection Platform of pesticide residues of Chinese traditional patent medicine in Guizhou Province was built to give the quality assurance and technical support for modern and international Chinese traditional patent medicine in Guizhou. Main content of the study are as follows :
1 The organochlorine pesticides residues were determined which from different major Chinese traditional patent medicine of Guizhou Province. The results showed that there have detected 52 organochlorine pesticides of 71 sample, and the detection rate of 73. 24%, the majority of samples pesticide residues is less than 0. Olmg/kg. According to Chinese Pharmacopoeia(2005 version) organochlorine pesticide residues of the limited standards, there is no excessive samples; referencing to "Green Trade Standards of Importing & Exporting Medicinal plants & Preparations" , over standard rate is 1.4%.
2 The Pyrethriods Pesticide residues were determined which from different major Chinese traditional patent medicine of Guizhou Province. To establish a method for determination Pyrethriods Pesticide in Chinese traditional patent medicine by the electron capture detector-capillary gas chromatography. The recoveries and RSD of Pyrethriods Pesticide were 78. 69%～113. 52%. The linear ranges were 0.10～5.0μg/mL It can be used to detect Pyrethriods Pesticide from Chinese traditional patent medicine. There were 25 of 71 sample was detected Pyrethriods Pesticide, and the detection rate is 35.21%. Referencing to "maximum residue limits of Tea in the European" , 71 samples of Chinese patent medicine did not exceed the standard.
3 The Organophosphorous Pesticide residues were determined which from different major Chinese traditional patent medicine of Guizhou Province. To establish a method for determination Organophosphorous Pesticide in Chinese traditional patent medicine by the pulsed flame photometric detector (PFPD)- gas chromatography, and the column was OV-1701 capillary column. all the samples were not detected of organophosphorus pesticide residues. This may be related to degradation period of organophosphorus pesticide is relatively short, the properties instability. Generally speaking, Chinese traditional patent medicine did not have organophosphorus pesticide.
4 To establish a method for determination Organochlorine pesticides in Chinese traditional patent medicine by -gas chromatography. The sample was extract with acetone , dichloromethane , GPC purification, and detected with electron capture detector (ECD). The recoveries of Organochlorine pesticides were 87. 21%～109. 54%. The detected limited were 0. 000182～0. 003295μg/mL. It can be used to detect Organochlorine pesticides from Chinese traditional patent medicine.
引文
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