2.8.13. PESTICIDE RESIDUES（农药残留） Definition. For the purposes of the Pharmacopoeia, a pesticide is any substance or mixture of substances intended for preventing, destroying or controlling any pest, unwanted species of plants or animals causing harm during or otherwise interfering with the production, processing, storage, transport or marketing of herbal drugs. The item includes substances intended for use as growth-regulators, defoliants or desiccants and any substance applied to crops either before or after harvest to protect the commodity from deterioration during storage and transport. 定义“根据药典的宗旨，农药是以任何物质或某些物质的混合物，以防止在草药的生产、加工、储存、运输和销售过程中使用的避免虫害的物质。改项目包括用在农作物收获前后的作生长调节剂、落叶剂、干燥剂以及在药品储存和运输中的保护剂。
Limits. Unless otherwise indicated in the monograph, the drug to be examined at least complies with the limits indicated in Table 2.8.13.-1. The limits applying to pesticides that are not listed in the table and whose presence is suspected for any reason comply with the limits set by European Community directives 76/895 and 90/642, including their annexes and successive updates. Limits for pesticides that are not listed in Table 2.8.13.-1 nor in EC directives are calculated using the following expression: 限量：除非专著中另有说明，草药的检测项目至少要按照表2.8.13-1进行。该表中未列出的农业检测项目，按照欧洲共同体指令76/895和90/895进行检查，包括其附表和更新的项目。表2.8.13-1和EC指令中没有列出的农药检测项目，按照下面的表达式进行计算：
If the drug is intended for the preparation of extracts, tinctures or other pharmaceutical forms whose preparation method modifies the content of pesticides in the finished product, the limits are calculated using the following expression : 如果该药物是制作提取物，在制作酊剂或其他药物剂型过程中有可能改变农药的含量，最终产品中农药的残留的计算方法按照下面的公式：
Higher limits can also be authorised, in exceptional cases, especially when a plant requires a particular cultivation method or has a metabolism or a structure that gives rise to a higher than normal content of pesticides. 在特殊情况下，可以允许更高的农药限度，特别是当一种草药需要特殊的种植方法，或产生代谢、或有特别的结构产生了高于正常含量的杀虫剂。
The competent authority may grant total or partial exemption from the test when the complete history (nature and quantity of the pesticides used, date of each treatment during cultivation and after the harvest) of the treatment of the batch is known and can be checked precisely. 当使用的药材有完整的历史记录时（包括使用农药的性质和数量，种植和收获中每次使用农药的时间），并且每批的记录都可以准确的进行检查时，主管机关可以全部或部分免除检测。
Sampling样品分析
Method. For containers up to 1 kg, take one sample from the total content, thoroughly mixed, sufficient for the tests. For containers between 1 kg and 5 kg, take three samples, equal in volume, from the upper, middle and lower parts of the container, each being sufficient to carry out the tests. Thoroughly mix the samples and take from the mixture an amount sufficient to carry out the tests. For containers of more than 5 kg, take three samples, each of at least 250 g from the upper, middle and lower parts of the container. Thoroughly mix the samples and take from the mixture an amount sufficient to carry out the tests. 方法：当包装容器达1kg，采取一个足以进行试验的样本，彻底混合。当样品的容量在1-5kg之间时，从上、中、下三个部位分别采取三个足以进行试验的样本。但样本的容量在5kg以上时，从上、中、下三个部位分别采取至少250g的样本进行试验，将三个样本混合，并采取足够的样品量进行试验。
Size of sampling. If the number (n) of containers is three or fewer, take samples from each container as indicated above under Method. If the number of containers is more than three, take samples from containers as indicated under Method, rounding up to the nearest unit if necessary. The samples are to be analysed immediately to avoid possible degradation of the residues. If this is not possible, the samples are stored in airtight containers suitable for food contact, at a temperature below 0 °C, protected from light. 样品数量：如果样品的容器小于或等于3个，按照上述方法从每个容器中采取样本。如果样品的容器多于三个，按照上述方法，采取 个容器中的样品，如有必要四舍五入到最接近的单位。样品最好马上进行分析，以免农药残留物发生降解。如果不能马上进行，样品密封、避光并低于零度保存。
Reagents. All reagents and solvents are free from any contaminants, especially pesticides, that might interfere with the analysis. It is often necessary to use special quality solvents or, if this is not possible, solvents that have recently been re-distilled in an apparatus made entirely of glass. In any case, suitable blank tests must be carried out. 试剂：所有试剂和溶剂不能受任何污染，特别是农药，以免干扰分析。通常需要使用特殊质量的溶剂，如果做不到这一点，最好将溶剂采用玻璃瓶进行重新蒸馏。在任何情况下，必须进行空白试验。
Apparatus. Clean the apparatus and especially glassware to ensure that they are free from pesticides, for example, soak for at least 16 h in a solution of phosphate-free detergent, rinse with large quantities of distilled water R and wash with acetone and hexane or heptane. 器具：清洁器具，特别是玻璃制品，以确保他们不受农药的污染，例如，至少在无磷洗涤剂中浸泡16个小时，然后用大量蒸馏水进行漂洗，再用丙酮和正己烷或正庚烷进行洗涤。
Qualitative and quantitative analysis of pesticide residues. 农药残留的定性和定量分析
The analytical procedures used are validated according to the regulations in force. In particular, they satisfy the following criteria : 使用的分析程序，验证根据该条例生效。特别是，当它们满足以下条件： — the chosen method, especially the purification steps, are suitable for the combination pesticide residue/substance to be analysed, and not susceptible to interference from co-extractives ; the limits of detection and quantification are measured for each pesticide-matrix combination to be analysed, 所选择的方法，特别是净化步骤，适合分析混合的农药残留/物质，而且不容易受到干扰，共同提取物的检测限和定量测量按每个农药矩阵组合进行分析
— between 70 per cent to 110 per cent of each pesticide is recovered, — 每个农药的回收率在70-110%之间 — the repeatability of the method is not less than the values indicated in Table 2.8.13.-2, — 方法的重复性不小于表2.8.13-2所列的数值 — the reproducibility of the method is not less than the values indicated in Table 2.8.13.-2, — 方法的重现性不小于表2.8.13-2所列的数值 — the concentration of test and reference solutions and the setting of the apparatus are such that a linear response is obtained from the analytical detector. — 检测浓度和参比溶液以及仪器的设定，根据检查分析应该是线性响应。
The following section is published for information. 下面一节是出版信息。
Test for pesticides农药检测 ORGANOCHLORINE, ORGANOPHOSPHORUS AND PYRETHROID INSECTICIDES 有机氯，有机磷及拟除虫菊酯类农药
The following methods may be used, in connection with the general method above. Depending on the substance being examined, it may be necessary to modify, sometimes extensively, the procedure described hereafter. In any case, it may be necessary to use, in addition, another column with a different polarity or another detection method (mass spectrometry...) or a different method (immunochemical methods...) to confirm the results obtained. 下列方法与上述的总方法相关。根据正在审议的实质内容，在将来可能会进行修改，或者会进行大部分的修改。在任何情况下，必须使用，此外，另一列具有不同极性或其他检测方法（质谱... ）或一个不同的方法（免疫组织化学方法... ） ，以确认所取得的成果。
This procedure is valid only for the analysis of samples of herbal drugs containing less than 15 per cent of water. Samples with a higher content of water may be dried, provided it has been shown that the drying procedure does not affect significantly the pesticide content.
To 10 g of the substance being examined, coarsely powdered, add 100 ml of acetone R and allow to stand for 20 min. Add 1 ml of a solution containing 1.8 μg/ml of carbophenothion R in toluene R. Homogenise using a high-speed blender for 3 min. Filter and wash the filter cake with two quantities, each of 25 ml, of acetone R. Combine the filtrate and the washings and heat using a rotary evaporator at a temperature not exceeding 40 °C until the solvent has almost completely evaporated. To the residue add a few millilitres of toluene R and heat again until the acetone is completely removed. Dissolve the residue in 8 ml of toluene R. Filter through a membrane filter (45 μm), rinse the flask and the filter with toluene R and dilute to 10.0 ml with the same solvent (solution A). 称取10g的检测样品，粉碎成粗粉，加入丙酮100ml，静止20min，加入1.8ug/ml的三硫磷-甲苯混合溶液1ml，高速搅拌3分钟，过滤，用丙酮洗涤滤纸两次，每次25ml。合并过滤液和洗涤液，采用旋转蒸发仪在低于40度的温度下进行旋转蒸发，直至溶剂基部完全消失。再加入几毫升的甲苯，继续回收至丙酮完全消除。残留物用8ml甲苯溶解，并用滤膜（45um）过滤，用甲苯冲洗蒸发瓶和过滤器，并稀释到10ml（溶液A）
。
2. PURIFICATION纯化
2.1. Organochlorine, organophosphorus and pyrethroid insecticides. Examine by size-exclusion chromatography (2.2.30). 有机氯，有机磷和拟除虫菊酯类农药。排阻色谱法检测（ 2.2.30 ） 。
The chromatographic procedure may be carried out using: 可进行使用下列色谱程序： — a stainless steel column 0.30 m long and 7.8 mm in internal diameter packed with styrene-divinylbenzene copolymer R (5 μm), — 不锈钢柱，长0.30米，内径7.8毫米，填充物：苯乙烯-二乙烯基苯共聚体（ 5微米） — as mobile phase toluene R at a flow rate of 1 ml/min. — 流动相：甲苯 ，流速：1 ml/min。
Performance of the column. Inject 100 μl of a solution containing 0.5 g/l of methyl red R and 0.5 g/l of oracet blue 2R R in toluene R and proceed with the chromatography. The column is not suitable unless the colour of the eluate changes from orange to blue at an elution volume of about 10.3 ml. If necessary calibrate the column, using a solution containing, in toluene R, at a suitable concentration, the insecticide to be analysed with the lowest molecular mass (for example, dichlorvos) and that with the highest molecular mass (for example, deltamethrin). Determine which fraction of the eluate contains both insecticides. 色谱柱性能：在色谱柱中注入100ul的甲苯溶液（包含0.5g/L的甲基红和0.5g/L的oracet blue 2R）。如果洗脱液在10.3ml的时候颜色由橙色变为蓝色，该色谱柱是可以使用的。 如果需要校正色谱柱，用甲苯在适当的浓度下进行研究，即可以分析最低分子量的杀虫剂（如：敌敌畏），又可以分析最高分子量的杀虫剂（如，溴氰菊酯）。并且确定每一部分洗脱液中包含的所洗脱的杀虫剂。
Purification of the test solution. Inject a suitable volume of solution A (100 μl to 500 μl) and proceed with the chromatography. Collect the fraction as determined above (solution B). Organophosphorus insecticides are usually eluted between 8.8 ml and 10.9 ml. Organochlorine and pyrethroid insecticides are usually eluted between 8.5 ml and 10.3 ml. 测试溶液的纯化：注入适当体积的溶液A（100ul-500ul），通过色谱柱。根据上述确定的部位进行收集（溶液B）。有机磷杀虫剂通常在8.8ml-10.9ml之间被洗脱，有机氯和拟除虫菊酯类农药通常8.5ml-10.3ml之间被洗脱。
2.2. Organochlorine and pyrethroid insecticides. In a chromatography column, 0.10 m long and 5 mm in internal diameter, introduce a piece of defatted cotton and 0.5 g of silica gel treated as follows : heat silica gel for chromatography R in an oven at 150 °C for at least 4 h. 2.2有机氯和拟除虫菊酯类农药 层析柱：长0.1m、内径5mm；填充一块脱脂棉花和0.5克硅胶，处理如下：在烘箱中150度加热硅胶层析柱至少4h。
Allow to cool and add dropwise a quantity of water R corresponding to 1.5 per cent of the mass of silica gel used; shake vigorously until agglomerates have disappeared and continue shaking for 2 h using a mechanical shaker. Condition the column using 1.5 ml of hexane R. Prepacked columns containing about 0.50 g of a suitable silica gel may also be used provided they are previously validated. 以滴的形式加入1.5%硅胶质量的水进行降温，大力振摇直至团聚力消失，然后采用机械振动2h。加入1.5ml的正己烷。可以使用一个含有0.5g硅胶的层析柱进行预实验。
Concentrate solution B in a current of helium for chromatography R or oxygen-free nitrogen R almost to dryness and dilute to a suitable volume with toluene R (200 μl to 1 ml according to the volume injected in the preparation of solution B). Transfer quantitatively onto the column and proceed with the chromatography using 1.8 ml of toluene R as the mobile phase. Collect the eluate (solution C). 将溶液B用氦气或无氧氮气干燥，并用甲苯稀释（200ul-1ml，根据溶液B注射的体积）。将溶液定量转移到色谱柱，并用1.8ml的甲苯作为流动相，收集洗脱液（溶液C）。
3. QUANTITATIVE ANALYSIS 3.定量分析 3.1. Organophosphorus insecticides. Examine by gas chromatography (2.2.28), using carbophenothion R as internal standard. It may be necessary to use a second internal standard to identify possible interference with the peak corresponding to carbophenothion. 3.1有机磷杀虫剂
Test solution. Concentrate solution B in a current of helium for chromatography R almost to dryness and dilute to 100 μl with toluene R. 测试溶液：溶液B用氦气流干燥，并用甲苯稀释至100ul
Reference solution. Prepare at least three solutions in toluene R containing the insecticides to be determined and carbophenothion at concentrations suitable for plotting a calibration curve. 对照品溶液：至少准备包含三个待测定的杀虫剂甲苯溶液和三硫磷溶液，以制作标准曲线。 The chromatographic procedure may be carried out using: 在进行分析时可选用： — a fused-silica column 30 m long and 0.32 mm in internal diameter the internal wall of which is covered with a layer 0.25 μm thick of poly (dimethyl) siloxane R, 毛细管柱，长30m，内径0.32mm，内径涂有0.25um厚的聚（二甲基）硅氧烷。
— hydrogen for chromatography R as the carrier gas. Other gases such as helium for chromatography R or nitrogen for chromatography R may also be used provided the chromatography is suitably validated. 采用氢气作为载运气体，如采用氦气或氮气需要提供验证方法。
— a phosphorus-nitrogen flame-ionisation detector or a atomic emission spectrometry detector, maintaining the temperature of the column at 80 °C for 1 min, then raising it at a rate of 30 °C/min to 150 °C, maintaining at 150 °C for 3 min, then raising the temperature at a rate of 4 °C/min to 280 °C and maintaining at this temperature for 1 min, and maintaining the temperature of the injector port at 250 °C and that of the detector at 275 °C. Inject the chosen volume of each solution. When the chromatograms are recorded in the prescribed conditions, the relative retention times are approximately those listed in Table 2.8.13.-3. Calculate the content of each insecticide from the peak areas and the concentrations of the solutions. 磷氮火焰电离探测器或原子发射光谱仪。程序升温：柱温度初始80 ℃，保持1分钟后，以每分钟30 ℃升至150℃ ，保持3分钟；再以每分钟4 ℃ 升至280 ℃ ，保持1分钟。进样口及检测器温度应分别保持为250℃和275℃。 在上述分析条件下，注入适量的供试品溶液和对照品溶液，拟测定农药的相对保留时间见表2.8.13-3。测定峰面积，计算供试品溶液中拟测定农药的浓度，并计算样品中农药的含量。
3.2. Organochlorine and pyrethroid insecticides. Examine by gas chromatography (2.2.28), using carbophenothion as the internal standard. It may be necessary to use a second internal standard to identify possible interference with the peak corresponding to carbophenothion 3.2有机氯和拟除虫菊酯类农药 气相色谱（ 2.2.28 ），用三硫磷作为内标物，可能需要第二个内标物，以确定可能的三硫磷干扰峰
Test solution. Concentrate solution C in a current of helium for chromatography R or oxygen-free nitrogen R almost to dryness and dilute to 500 μl with toluene R. 测试溶液：采用氦色谱或无氧铜氮浓缩溶液C至干燥，用甲苯稀释至500ul。
Reference solution. Prepare at least three solutions in toluene R containing the insecticides to be determined and carbophenothion at concentrations suitable for plotting a calibration curve. 对照品溶液：至少准备含有三个待测定的杀虫剂的甲苯溶液和三硫磷溶液，以制作标准曲线。
The chromatographic procedure may be carried out using: 在进行分析时可选用： — a fused silica column 30 m long and 0.32 mm in internal diameter the internal wall of which is covered with a layer 0.25 μm thick of poly(dimethyl)(diphenyl)siloxane R, 毛细管色谱柱，长30m，内径0.32mm，内径覆盖0.25um厚的聚（二甲基）硅氧烷
— hydrogen for chromatography R as the carrier gas. Other gases such as helium for chromatography R or nitrogen for chromatography R may also be used, provided the chromatography is suitably validated, 采用氢气作为载运气体，如采用氦气或氮气需要提供验证方法。
— an electron-capture detector, 电子捕获检测器
— a device allowing direct cold on-column injection, maintaining the temperature of the column at 80 °C for 1 min, then raising it at a rate of 30 °C/min to 150 °C, maintaining at 150 °C for 3 min, then raising the temperature at a rate of 4 °C/min to 280 °C and maintaining at this temperature for 1 min, and maintaining the temperature of the injector port at 250 °C and that of the detector at 275 °C. Inject the chosen volume of each solution. When the chromatograms are recorded in the prescribed conditions, the relative retention times are approximately those listed in Table 2.8.13.-4. Calculate the content of each insecticide from the peak areas and the concentrations of the solutions.
2.8.13. PESTICIDE RESIDUES（农药残留） Definition. For the purposes of the Pharmacopoeia, a pesticide is any substance or mixture of substances intended for preventing, destroying or controlling any pest, unwanted species of plants or animals causing harm during or otherwise interfering with the production, processing, storage, transport or marketing of herbal drugs. The item includes substances intended for use as growth-regulators, defoliants or desiccants and any substance applied to crops either before or after harvest to protect the commodity from deterioration during storage and transport. 定义“根据药典的宗旨，农药是以任何物质或某些物质的混合物，以防止在草药的生产、加工、储存、运输和销售过程中使用的避免虫害的物质。改项目包括用在农作物收获前后的作生长调节剂、落叶剂、干燥剂以及在药品储存和运输中的保护剂。 这段话是对农药的定义，我认为上面红色标记的那句是对any pest的解释，所以我的翻译是：农药是用来预防、破坏或控制有害物质的任一物质或物质的混合物，有害物质包括草药的生产、加工、储存或销售过程中出现的不必要种类的植物或引起损害或其他方面干扰的动物。该项目包括用作生长调节剂、落叶剂或干燥剂的物质以及在农作物收获前后用来保护物品在储存和运输中变质的物质。
Limits. Unless otherwise indicated in the monograph, the drug to be examined at least complies with the limits indicated in Table 2.8.13.-1. The limits applying to pesticides that are not listed in the table and whose presence is suspected for any reason comply with the limits set by European Community directives 76/895 and 90/642, including their annexes and successive updates. Limits for pesticides that are not listed in Table 2.8.13.-1 nor in EC directives are calculated using the following expression: 限量：除非专著中另有说明，草药的检测项目至少要按照表2.8.13-1进行。该表中未列出的农业检测项目，按照欧洲共同体指令76/895和90/895进行检查，包括其附表和更新的项目。表2.8.13-1和EC指令中没有列出的农药检测项目，按照下面的表达式进行计算 红色部分译成“所检测的药品至少应符合表2.8.13-1中所规定的限度”会不会更符合原文一些？
If the drug is intended for the preparation of extracts, tinctures or other pharmaceutical forms whose preparation method modifies the content of pesticides in the finished product, the limits are calculated using the following expression : 如果该药物是制作提取物，在制作酊剂或其他药物剂型过程中有可能改变农药的含量，最终产品中农药的残留的计算方法按照下面的公式：
The competent authority may grant total or partial exemption from the test when the complete history (nature and quantity of the pesticides used, date of each treatment during cultivation and after the harvest) of the treatment of the batch is known and can be checked precisely. 当使用的药材有完整的历史记录时（包括使用农药的性质和数量，种植和收获中每次使用农药的时间），并且每批的记录都可以准确的进行检查时，主管机关可以全部或部分免除检测。
我的社区
签到
赛默飞实验室产品焕新计划有奖调研！
【七月征文】不一YOUNG实验“猿”
报名开启：ICS2024第十三届光谱网络会议！
推荐收藏！盘点中药材及饮片检测解决方案
