【作者】 李申杰；

【导师】 万益群；

【作者基本信息】 南昌大学 ， 分析化学， 2007， 硕士

【摘要】 农药的发明和使用是种植行业的极大重点突破之一，大大地提高了农作物的产量，与此同时也带来了一些负面影响。例如，由于人们在种植中草药的过程中大量喷洒农药，给中药材造成污染，给人民身体健康带来隐患，成为影响生态环境的主要污染物。此外，重金属也是危害人们身体健康的重要因素之一。因此尽快建立中药中农药残留及重金属元素含量检测方法和限量标准，对保证人们用药安全具有积极的意义。本文在查阅国内外大量文献的基础上，系统地对中药中多种类型农药及重金属测定进行探索，建立了中药中多种类型的农药残留和重金属元素的同时测定分析方法。具体内容如下：1．建立了微波辅助提取、气相色谱-质谱法测定中药中21种有机磷和氨基甲酸酯类农药残留的分析方法。以乙腈-丙酮(3：7，V／V)为提取剂，经弗罗里硅土及中性氧化铝层析柱净化、气相色谱-质谱法同时检测中药中21种有机磷和氨基甲酸酯类农药的残留量，农药混标在0.01～1.0μg／mL的浓度范围内线性良好，在0.5、0.1、0.05μg／mL三个水平添加平均回收率分别为86.5％～110.6％、81.2％～108.3％和72.9％～122.3％，相对标准偏差分别为2.6％～8.3％、4.6％～9.7％和2.3％～10.7％。采用选择离子模式检测排除了干扰，提高了选择性，取得了较好的效果。2．建立了中药材中28种有机氯及拟除虫菊酯类农药残留的毛细管气相色谱测定方法，以乙腈为提取剂，微波辅助萃取，层析柱法净化。28种农药中有机氯农药的检测限0.001～0.008μg／mL，拟除虫菊酯类农药检测限0.005～0.024μg／mL，28种有机农药的线性相关系数为0.9984～0.9999。该方法具有很好的选择性、重现性，适合于中药材中有机氯及拟除虫菊酯类农药残留的分析。3．建立了中药材中12种重金属元素的测定方法。采用微波消解，等离子体原子发射光谱法测定。12种重金属在1.0、2.0 mg／L两个水平添加的回收率分别为98.4％～107.4％和93.1％～103.8％。相对标准偏差分别为2.19％～4.22％和2.08％～4.44％。可以满足实际样品的分析要求，对中草药中重金属含量检测具有借鉴意义。更多还原

【Abstract】 The invention of pesticides has been played a very important role in agriculture.it greatly improved the output of crops. At the same time, some damages came. Forexample, Chinese herbal medicine(CHM), as a special plant, was polluted in growingtime, because people used too much pesticides in order to prevent dieases, it isharmful to our health and our environment. CHMs have a high risk of contaminationof pesticides. Besides,heavy metals are also harmful to people’s health. So it is veryimportant to strengthen the study on determination of pesticide residues and heavymetals in CHMs.Referred to a lot of literatures, this paper explored a series ofexperimental methods such as extraction, purification and analytical techniques insamples. Methods for the determination of multi-residue pesticides and heavy metalsin Chinese herbal medicines were investigated. The main contains as follows:1. A method to determine 21 organophosphorous and carbamate pesticideresidues in Chinese herbal medicine was established. Pesticide residues wereextracted from CHMs samples with a mixture solvent of acetonitril:aceton(3:7).Extracts were cleaned up with a column filled with Florisil and neutral alumiumoxide, and determined by gas chromatography-mass spectrometry. The recoveriesobtained from CHMs at three concentration levels, 0.5,0.1 and 0.05 mg of pesticideper kg sample, were in the ranges of 86.5％～110.6％,81.2％～108.3％and 72.9％～122.3％, with relative standard deviations of 2.6％～8.3％,4.6％～9.7％and 2.3％～10.7％. Detection sensitivity can be significantly increased and interference fromimpurities can be excluded by using selective ionic monitoring technique. Themethod was proved to be effective and practical.2. A method was developed for the determination of 28 organochlorine andpyrethroid pesticide residues in CHMs by gas chromatography and electron-capturedetection. Pesticide residues were extracted by microwave extraction with acetonitrile,and cleaned up with a column filled with florisil and neutral aluminum. Detectionlimits of organochlorine and pyrethroid pesticides were 0.001～0.008 and 0.005～ 0.024 mg of per kg sample, respectively. The range of correlation coefficient was0.9984～0.9999. The method was proved to be effective and practical.3. A method to determine 12 heavy metals in CHMs was investigated. Sampleswere digested by microwave, and determined by ICP-AES. The rescoveries at twoconcentration levels, 1.0 and 2.0 mg of heavy metals per kg sample were in the rangsof 98.2％～105.7％and 94.5％～103.1％, with relative standard deviation of2.19％～4.22％and 2.08％～4.44％. The method could be used for a heavy metalstest, it is useful for the determination of heavy metals in CHMs.更多还原