中药中100种农药GC/GC-MSn测定方法研究
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摘要
本研究分别以根茎类、花类、叶类和果实类药材为研究对象,以其中易残留的、各国各地区官方组织规定的植物药中需检测的农药种类为分析目标,综合运用了超声提取、固相萃取小柱净化、气相色谱检测技术和气相色谱质谱联用检测技术建立了中药材这一复杂基质中的农药多残留测定方法,这些方法弥补了以往中药中农药多残留检测分析方法的不足,为不同层次的科研单位、检测单位的相关工作人员提供参考。本文主要研究成果如下：
(1)建立了果实类药材中50种有机氯类及菊酯类农药GC-ECD检测的分析方法。此方法仪器简便,适用于大部分分析实验室的操作条件,因此该技术方法与目前大多的中药中农药多残留检测方法相比适用性更广。
方法考察结果表明,各农药标准品在三个不同浓度下,在枸杞样品中的添加回收率都在75.1%-111.1%范围内,RSD<15.0%,符合农药残留检测的要求。同时考察了其它40种果实类药材的146个样品,结果表明除瓜蒌、柏子仁、南五味子、紫苏子、补骨脂、乌梅、苦杏仁、益智仁这8种药材以外,其它32种药材均适用于所建立的农药多残留检测的分析方法。测定了21个枸杞样品,结果有11个样品有农药残留检出,检出农药以菊酯类农药为主,但残留量均低于0.2 mg/kg。所测其它样品,检出农药的残留量均低于0.05 mg/kg。检出的农药品种以有机氯为主,其中五氯硝基苯的检出率最高为10.3%。通过所测样品表明目前国内市场的大部分果实类药材的农药残留量较少,果实类的药材质量在农药残留方面较好。
(2)完成了中药中100种农药GC-MS-SIM和GC-MS-MS多残留检测方法在根类、花类和叶类中药材上方法适用性考察。结果表明,添加回收实验的GC-MS-SIM和GC-MS-MS检测,所有的回收率总体较好,除个别农药回收率偏低以外,大部分的结果都在70.0%-120.0%范围内,RSD≤15.0%,符合农药残留检测的要求。通过对根类药材、花类药材及叶类药材的248个样品进行测定和考察,考察结果表明所建立的100种农药多残留GC-MSn检测分析方法均适用于这248个样品,表明该方法在中药材中具有广泛的适用性。可为有实验条件的相关科研单位和检测单位做中药中农药多残留的快速检测和筛查提供参考。测定了28个人参样品,检出农药以有机氯类农药为主,如六六六、五氯硝基苯、甲基五氯苯基硫醚、腐霉利等,其中4个样品中的五氯硝基苯残留量超出2010版中国药典的限量标准(五氯硝基苯≤0.2 mg/kg),其它所有检出的农药残留量均低于0.2 mg/kg。测定了32个菊花样品,样品检出农药以有机磷类农药为主如乙酰甲胺磷、克百威、毒死蜱等。测定的6个枇杷叶样品,其中有3个样品检出虫螨畏、克百威、西玛津和毒死蜱的残留,但检出浓度均低于0.05 mg/kg。
In this study, the pesticides contaminations of Chinese medicines vulnerability to pollution, including fruit, root, flower and leaf herbs, have been investigated. The target pesticides residues were selected based on the suggestion from various official documents. By comprehensive using of ultrasonic extraction, solid phase extraction, GC and GC-MS technology, the pesticide residues in the complex matrix of traditional Chinese medicines had been determined. This study was preformed to develop methods to make up for the lack of the past. The aim is to provide reference for the related scientists in different levels of scientific research institutions, testing organizations.The main results of this study are described as follows:
(1) Established a method to detect 50 kinds of organochlorine and pyrethrin pesticides in fruit Chinese materials by GC-ECD. This method is easy to perform, most of the instrument analysis lab can satisfy the operation condition, therefore the technical methods more applicable.
The recoveries obtained for all three target compounds ranged from 75.1% toll 1.1% with RSDs lower than 15%. Examine the 40 kind of fruit Chinese materials in addition to good other than fructus trichosanthis, fructus mume, fructus schisandrae, semen armeniacae amarum, fructus psoraleae, fructus alpiniae oxyphyllae applicability. The method was applied to the determination of the studied pesticides in 21 batches of Chinese wolfberry samples. The results demonstrated that the pesticides were detected only in 11 batches of samples with relative low amount, lower than 0.2 mg/kg. Results show that organochlorine pesticides were most detected in the most of studied samples, their contents lower than 0.05mg/kg. The highest content for PCNB was 10.3%. These results demonstrated that the most of fruit herbs in the domestic market contain relative lower residues, therefore, have high quality.
(2) Conducted the evaluation of GC-MS-SIM and GC-MS-MS methods for determination 100 kinds of pesticides residue in Chinese medicines. The two methods were proved to be applicable in root class, flowery and leafy herbs.
Three representative herbs, including Chinese ginseng (the root herb), Chrysanthemum (flower herb) and loquat (leaf herb) were used for extraction recovery test in the GC-MS-SIM and GC-MS-MS methods. The results showed that the recovery for most of the pesticides from three herbs were satisfactory and ranged from 75.0% to 125.0%, with RSD less than 15.0%, except for several pesticides with lower or higher recovery rate. This showed that the methods met the analytical requirements for determination of pesticide residues. In the study,28 batches of ginseng samples were measured for determination of pesticide residues. Most of these samples contained organochlorine pesticides, and 4 of them contained relative higher content of PCNB residue, which were higher than the control limits in the Chinese Pharmacopoeia 2010 (PCNB< 0.2 mg/kg). Except for organochlorine pesticides, most of the tested samples had low content of pesticide residues. Thirty two Chrysanthemum samples were measured for detection of residues, which were found mainly phosphorus pesticides. Six loquat leaf samples were assayed for detection of residues, and three of these samples contained organophosphorus pesticides, including methacrifos, carbofuran, simazine and and chlorpyrifos, with lower contents less than 0.05 mg/kg.
(1)建立了果实类药材中50种有机氯类及菊酯类农药GC-ECD检测的分析方法。此方法仪器简便,适用于大部分分析实验室的操作条件,因此该技术方法与目前大多的中药中农药多残留检测方法相比适用性更广。
方法考察结果表明,各农药标准品在三个不同浓度下,在枸杞样品中的添加回收率都在75.1%-111.1%范围内,RSD<15.0%,符合农药残留检测的要求。同时考察了其它40种果实类药材的146个样品,结果表明除瓜蒌、柏子仁、南五味子、紫苏子、补骨脂、乌梅、苦杏仁、益智仁这8种药材以外,其它32种药材均适用于所建立的农药多残留检测的分析方法。测定了21个枸杞样品,结果有11个样品有农药残留检出,检出农药以菊酯类农药为主,但残留量均低于0.2 mg/kg。所测其它样品,检出农药的残留量均低于0.05 mg/kg。检出的农药品种以有机氯为主,其中五氯硝基苯的检出率最高为10.3%。通过所测样品表明目前国内市场的大部分果实类药材的农药残留量较少,果实类的药材质量在农药残留方面较好。
(2)完成了中药中100种农药GC-MS-SIM和GC-MS-MS多残留检测方法在根类、花类和叶类中药材上方法适用性考察。结果表明,添加回收实验的GC-MS-SIM和GC-MS-MS检测,所有的回收率总体较好,除个别农药回收率偏低以外,大部分的结果都在70.0%-120.0%范围内,RSD≤15.0%,符合农药残留检测的要求。通过对根类药材、花类药材及叶类药材的248个样品进行测定和考察,考察结果表明所建立的100种农药多残留GC-MSn检测分析方法均适用于这248个样品,表明该方法在中药材中具有广泛的适用性。可为有实验条件的相关科研单位和检测单位做中药中农药多残留的快速检测和筛查提供参考。测定了28个人参样品,检出农药以有机氯类农药为主,如六六六、五氯硝基苯、甲基五氯苯基硫醚、腐霉利等,其中4个样品中的五氯硝基苯残留量超出2010版中国药典的限量标准(五氯硝基苯≤0.2 mg/kg),其它所有检出的农药残留量均低于0.2 mg/kg。测定了32个菊花样品,样品检出农药以有机磷类农药为主如乙酰甲胺磷、克百威、毒死蜱等。测定的6个枇杷叶样品,其中有3个样品检出虫螨畏、克百威、西玛津和毒死蜱的残留,但检出浓度均低于0.05 mg/kg。
In this study, the pesticides contaminations of Chinese medicines vulnerability to pollution, including fruit, root, flower and leaf herbs, have been investigated. The target pesticides residues were selected based on the suggestion from various official documents. By comprehensive using of ultrasonic extraction, solid phase extraction, GC and GC-MS technology, the pesticide residues in the complex matrix of traditional Chinese medicines had been determined. This study was preformed to develop methods to make up for the lack of the past. The aim is to provide reference for the related scientists in different levels of scientific research institutions, testing organizations.The main results of this study are described as follows:
(1) Established a method to detect 50 kinds of organochlorine and pyrethrin pesticides in fruit Chinese materials by GC-ECD. This method is easy to perform, most of the instrument analysis lab can satisfy the operation condition, therefore the technical methods more applicable.
The recoveries obtained for all three target compounds ranged from 75.1% toll 1.1% with RSDs lower than 15%. Examine the 40 kind of fruit Chinese materials in addition to good other than fructus trichosanthis, fructus mume, fructus schisandrae, semen armeniacae amarum, fructus psoraleae, fructus alpiniae oxyphyllae applicability. The method was applied to the determination of the studied pesticides in 21 batches of Chinese wolfberry samples. The results demonstrated that the pesticides were detected only in 11 batches of samples with relative low amount, lower than 0.2 mg/kg. Results show that organochlorine pesticides were most detected in the most of studied samples, their contents lower than 0.05mg/kg. The highest content for PCNB was 10.3%. These results demonstrated that the most of fruit herbs in the domestic market contain relative lower residues, therefore, have high quality.
(2) Conducted the evaluation of GC-MS-SIM and GC-MS-MS methods for determination 100 kinds of pesticides residue in Chinese medicines. The two methods were proved to be applicable in root class, flowery and leafy herbs.
Three representative herbs, including Chinese ginseng (the root herb), Chrysanthemum (flower herb) and loquat (leaf herb) were used for extraction recovery test in the GC-MS-SIM and GC-MS-MS methods. The results showed that the recovery for most of the pesticides from three herbs were satisfactory and ranged from 75.0% to 125.0%, with RSD less than 15.0%, except for several pesticides with lower or higher recovery rate. This showed that the methods met the analytical requirements for determination of pesticide residues. In the study,28 batches of ginseng samples were measured for determination of pesticide residues. Most of these samples contained organochlorine pesticides, and 4 of them contained relative higher content of PCNB residue, which were higher than the control limits in the Chinese Pharmacopoeia 2010 (PCNB< 0.2 mg/kg). Except for organochlorine pesticides, most of the tested samples had low content of pesticide residues. Thirty two Chrysanthemum samples were measured for detection of residues, which were found mainly phosphorus pesticides. Six loquat leaf samples were assayed for detection of residues, and three of these samples contained organophosphorus pesticides, including methacrifos, carbofuran, simazine and and chlorpyrifos, with lower contents less than 0.05 mg/kg.
引文
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