六种绿叶蔬菜中典型农药残留规律及代表作物研究
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摘要
作物上农药非法使用、不正确使用、超范围使用和缺乏限量标准等问题是农产品和食品安全的核心问题。根据作物形态学特点和农药残留分布规律的不同,将作物进行适当分类和分组,选取同一组和亚组中具有相似形态和残留行为并且具有经济价值的作物作代表作物,对典型代表作物进行规范田间残留试验并对残留数据进行外推是一条科学有效的解决品种繁多的作物包括小作物上缺少农药登记和无农药残留限量标准的有效途径。
本研究建立了甲基托布津、多菌灵、甲霜灵、精吡氟禾草灵、嘧菌酯、噻嗪酮、杀扑磷、噻虫嗪、腐霉利、毒死蜱、高效氯氟氰菊酯、高效氯氰菊酯12种农药在小白菜(pakchoi)、小油菜(rape)、茼蒿(crown daisy)、苋菜(amaranth)、菠菜(spinach)、叶用莴苣(lettuce)、芹菜(celery)中的QuEChERS提取净化方法,其中甲基托布津、多菌灵、甲霜灵、精吡氟禾草灵、嘧菌酯、噻嗪酮、杀扑磷、噻虫嗪和腐霉利用LC-MS/MS测定,毒死蜱、高效氯氟氰菊酯和高效氯氰菊酯用GC-ECD检测。所有分析物在各基质中标准曲线的线性相关系数在0.991-1.00之间,线性范围在0.001-10.0mg/L之间。12种农药的添加回收率在60.1-118.6%范围内,RSD在1.1-13.9%之间,LOQ范围为0.01-0.08mg/kg范围内。该方法适用七种叶菜中12种农药的检测。
为选取绿叶蔬菜的代表作物,并为建立农药残留限量标准所采用,对甲基托布津、甲霜灵、精毗氟禾草灵、毒死蜱、高效氯氰菊酯在小白菜、油菜、茼蒿、苋菜、菠菜、叶用莴苣上进行三地田间残留试验。结果表明在相同的施药剂量下,菠菜或苋菜的原始沉积量、最大残留量更高,在相同的安全间隔期时菠菜或苋菜中残留量相对也较高。菠菜或苋菜被选作绿叶蔬菜的代表作物。为了验证所选代表作物的是否合适,进行了嘧菌酯、精吡氟禾草灵、噻嗪酮、杀扑磷、噻虫嗪、腐霉利和高效氯氰菊酯在六种绿叶蔬菜上三地的田间试验,同样比较农药的消解动态、原始沉积量、最大残留量和最终残留。除茼蒿中部分农药的最终残留量相对较高外,其他试验结果均无差异。从农药消解动态、原始沉积量、最大残留量、最终残留量等几个方面综合考虑,本研究结果表明菠菜或苋菜可作为绿叶蔬菜的代表作物。
为考察不同生长季节对农药残留规律的影响,对甲基硫菌灵等5种农药在小白菜、油菜、茼蒿、苋菜、菠菜、叶用莴苣上进行了两季(夏季：5-7月份；秋季：8-10月份)田间试验。结果表明在相同的施药剂量下,大部分农药秋季的原始沉积量、最大残留量大于夏季的原始沉积量和最大残留量。在相同的收获间隔期时,石家庄样品中超过85%农药秋季的残留量高于夏季残留量,北京样品几乎所有农药残留量均高于夏季残留量。为验证以上试验结果,对嘧菌酯、精吡氟禾草灵、噻嗪酮、杀扑磷、噻虫嗪、腐霉利和高效氯氰菊酯在石家庄、北京和南京进行一年两季的残留试验。试验结果表明,在相同的施药剂量下大部分农药秋季原始沉积量、最大残留量高于夏季的原始沉积量和最大残留量；超过70%样品中农药秋季的残留量高于夏季残留量。方差分析结果表明不同生长季节对农药原始沉积量和半衰期的影响较大,对最终残留量影响较小。
为考察不同施药次数对农药残留规律的影响,对嘧菌酯、精吡氟禾草灵、噻嗪酮、杀扑磷、噻虫嗪、腐霉利和高效氯氰菊酯在芹菜上进行一年两季(夏季和秋季)的残留实验,试验设计施药一次和两次,从农药消解动态、原始沉积量、最大残留量、最终残留量等几个方面考察不同施药次数对农药残留行为的影响。结果表明,施药间隔7d时,夏季试验时约64%的农药施药两次时半衰期比施药一次时半衰期长,秋季试验时越50%的农药施药两次时半衰期比施药一次时半衰期长。石家庄夏季试验结果表明,芹菜施药两次时嘧菌酯、噻嗪酮、杀扑磷、噻虫嗪和高效氯氰菊酯的原始沉积量比施药一次时高；秋季试验施药两次时7种农药的原始沉积量均比施药一次要高,而且原始沉积量增加的幅度比夏季试验时要高很多,特别是嘧菌酯和高效氯氰菊酯。北京的试验结果跟石家庄一致,施药两次时农药的原始沉积量比施药一次时高(夏季试验嘧菌酯除外),而且秋季试验时原始沉积量增长比例比夏季施药时要高。夏季试验时约60%的农药施药两次时,最终残留量较施药一次有升高；而同样的施药剂量条件下秋季试验时超过90%的农药施药两次时,农药的最终残留量比施药一次时残留量更高。方差分析结果表明不同施药次数时芹菜中农药的原始沉积量、半衰期和最终残留量均无显著差异。
对六种绿叶蔬菜中农药残留进行了膳食摄入风险评估。从多菌灵等5种农药慢性风险评估结果来看,菠菜和苋菜或叶用莴苣的慢性风险较高；从嘧菌酯等7种农药慢性风险评估结果来看,菠菜和苋菜或茼蒿的慢性风险较高。多菌灵等5种农药急性风险评估结果表明菠菜和苋菜中急性风险比较高,嘧菌酯等7种农药急性风险评估结果也表明菠菜和苋菜中急性风险较高。膳食摄入风险评估综合了农药田间试验残留数据和食物的摄入水平,从风险评估结果来看,菠菜或苋菜可作为绿叶蔬菜的代表作物。
Ilegal usage, incorrect usage of pesticides, pesticides application out of the label, and the lack of maximum residue limits are the core issues of agricultural products and food safety. Crops are classified and grouped accourding to their morphology and residue characteristics, representative commodities are chosen based on their commercial importance and the similarity of their morphology and residue characteristics to other related commodities in the group or suboup. Supervised field residue trials of representative commodities will be conducted according to good agriculture production, and the residues datas could be used in the residue extrapolation, which is a scientific and effective solution to resolve relative problems such as lack of pesticide registration on minor crop and the absence of maximum residue limits.
In this study, a multi-residue method was built to determine of thiophanate-methyl, carbendazim, metalaxyl, fluazifop-P-butyl, azoxystrobin, buprofezin, methidathion, thiamethoxam, procymidone, chlorpyrifos, lambda-cyhalothrin, beta-cypermethrin in pakchoi, rape, crown daisy, amaranth, spinach, lettuce and celery. A quick, easy, cheap, effective, rugged and safe (QuEChERS) method was used in*sample preparation, thiophanate-methyl, carbendazim, metalaxyl, fluazifop-P-butyl, azoxystrobin, buprofezin, methidathion, thiamethoxam and procymidone were detected by liquid chromatography tandem mass spectrometry (LC-MS/MS), chlorpyrifos, lambda-cyhalothrin and beta-cypermethrin were determined by gas chromatography with electron capture detector (GC-ECD). The limits of quantification (LOQ) in all leafy vegetables were in the range of0.001-0.08mg/kg for all analytes and the average recoveries of all pesticides ranged from60.1%to118.6%. Good linearity was found for all pesticides with cofficients between0.991and1.00in a range of0.001-10.0mg/kg. The developed method was successfully used to determine the12pesticide residues in seven leafy vegetables.
To select representative commodities in leafy green vegetables and for adorption in establishment of maximum residue limits of pesticides, supervised field residue trails of thiophanate-methyl, fluazifop-P-butyl, metalaxyl, chlorpyrifos and lambda-cyhalothrin on six leafy green vegetables including pakchoi, rape, crown daisy, amaranth, spinach and lettuce were designed and conducted in three places. It was found that almost all initial concentrations and maximal concentrations of pesticides in spinach and/or amaranth were higher than others with the same application dose, and the final residues for most pesticides in shinach and/or amaranth at the same preharvest interval (PHI) were higher. Spinach and/or amaranth were selected as representative crop in leafy green vegetables. In order to verify the accuracy of representative commodities selected, supervised field residue trials of azoxystrobin, fluazifop-P-butyl, buprofezin, methidathion, thiamethoxam, procymidone, beta-cypermethrin in the six leaf vegetables were conducted in three places. Initial concentrations, maximal concentrations and final residues were also used to compare. In addition to the part of higher final residues in crown daisy, the other results were consistent. In consideration of residue dynamics, initial concentrations and final residues, spinach and/or amaranth were recommended to select as representative commodities in leafy green vegetables.
To investigate the influence of different planting seasons on the dissipation of pesticides, supervised field residue trails of thiophanate-methyl, metalaxyl, fluazifop-P-butyl, chlorpyrifos and lambda-cyhalothrin on six leafy green vegetables including pakchoi, rape, crown daisy, amaranth, spinach and lettuce were designed and conducted at two planting seasons (summer:between May and July; autumn:between August and October) in three places. The results showed that initial concentrations and maximal concentrations of most pesticides in six leafy green vegetables at autumn were higher that at summer. More than85%samples contained more pesticide residues at autumn at the same PHI in Shijiazhuang, and almost all samples had higher concentrations of pesticides at autumn at same PHI in Beijing. In order to verify the conclusion above, supervised field residue trails of azoxystrobin, fluazifop-P-butyl, buprofezin, methidathion, thiamethoxam, procymidone, beta-cypermethrin in the six leafy green vegetables were conducted at two planting seasons in Shijiazhuang, Beijing and Nanjing. For most pesticides, the initial concentrations and maximal concentrations at autumn were higher than that at summer with the same spray dose More than70%samples contained more pesticide residues at autumn at the same PHI. Analysis variance results showed that initial concentrations and half-lives of pesticides were influced by different planting seasons in a larger degree than the final residues.
In order to investigate the effect of different spraying times on pesticide residues, supervised field residue trails of azoxystrobin, fluazifop-P-butyl, buprofezin, methidathion, thiamethoxam, procymidone, beta-cypermethrin in celery were conducted at two planting seasons. The experiments were designed for spraying one time and two times. Initial concentrantions, maximal concentrations and final concentrations of pesticides were considered in data analysis. The results of the experiments showed that half-lives of about64%pesticides were longer when sprayed two times (spraying pesticide interval was7days) than that sprayed one time at summer, and half-lives of about50%pesticides were longer when sprayed two times at autumn. The initial concentrations of azoxystrobin, buprofezin, methidathion, thiamethoxam, beta-cypermethrin in celery when spraying two times were higher than that when spraying one time at summer in Shijiazhuang, the initial concentrations of the seven pesticides when spraying two times were higher than that spraying one time at autumn, and the increase was higher at autumn especially to azoxystrobin and beta-cypermethrin. The results of Beijing were consistent with that of Shijiazhuang, initial concentrations of pesticides when spraying two times were higher than that when spraying one time in Beijing in addition to the azoxystrobin at summer. Approximately60%samples contained more pesticide residues when spraying two times at summer, while more than90%samples had higher concentrations of pesticides when spraying two times at autumn. There were no significant differences in initial concentrations, half-lives and final residues in celery with different spraying times.
The dietary risk assessment of pesticides in six leafy green vegetables was conducted. The chronic assessment results of five pestides (carbendazim etc.) demonstrated that chronic dietary risk of spinach and amaranth (or leaf lettuce) was much higher; and the chronic assessment results of seven pesticides (azoxystrobin etc.) indicated that chronic dietary risk of spinach and amaranth (or crown daisy) was much higher. The acute assessment results of five pestides (carbendazim etc.) showed that acute dietary risk of spinach and/or amaranth was higher; and acute assessment results of seven pesticides (azoxystrobin etc.) presented that the acute dietary risk of spinach and/or amaranth was higher. Risk assessment is a comprehensive indicator in that it reflects the field experiment results and the dietary intake at same time. Spinach and/or amaranth could be recommended to select as representative commodities in according to the risk assessment results.
本研究建立了甲基托布津、多菌灵、甲霜灵、精吡氟禾草灵、嘧菌酯、噻嗪酮、杀扑磷、噻虫嗪、腐霉利、毒死蜱、高效氯氟氰菊酯、高效氯氰菊酯12种农药在小白菜(pakchoi)、小油菜(rape)、茼蒿(crown daisy)、苋菜(amaranth)、菠菜(spinach)、叶用莴苣(lettuce)、芹菜(celery)中的QuEChERS提取净化方法,其中甲基托布津、多菌灵、甲霜灵、精吡氟禾草灵、嘧菌酯、噻嗪酮、杀扑磷、噻虫嗪和腐霉利用LC-MS/MS测定,毒死蜱、高效氯氟氰菊酯和高效氯氰菊酯用GC-ECD检测。所有分析物在各基质中标准曲线的线性相关系数在0.991-1.00之间,线性范围在0.001-10.0mg/L之间。12种农药的添加回收率在60.1-118.6%范围内,RSD在1.1-13.9%之间,LOQ范围为0.01-0.08mg/kg范围内。该方法适用七种叶菜中12种农药的检测。
为选取绿叶蔬菜的代表作物,并为建立农药残留限量标准所采用,对甲基托布津、甲霜灵、精毗氟禾草灵、毒死蜱、高效氯氰菊酯在小白菜、油菜、茼蒿、苋菜、菠菜、叶用莴苣上进行三地田间残留试验。结果表明在相同的施药剂量下,菠菜或苋菜的原始沉积量、最大残留量更高,在相同的安全间隔期时菠菜或苋菜中残留量相对也较高。菠菜或苋菜被选作绿叶蔬菜的代表作物。为了验证所选代表作物的是否合适,进行了嘧菌酯、精吡氟禾草灵、噻嗪酮、杀扑磷、噻虫嗪、腐霉利和高效氯氰菊酯在六种绿叶蔬菜上三地的田间试验,同样比较农药的消解动态、原始沉积量、最大残留量和最终残留。除茼蒿中部分农药的最终残留量相对较高外,其他试验结果均无差异。从农药消解动态、原始沉积量、最大残留量、最终残留量等几个方面综合考虑,本研究结果表明菠菜或苋菜可作为绿叶蔬菜的代表作物。
为考察不同生长季节对农药残留规律的影响,对甲基硫菌灵等5种农药在小白菜、油菜、茼蒿、苋菜、菠菜、叶用莴苣上进行了两季(夏季：5-7月份；秋季：8-10月份)田间试验。结果表明在相同的施药剂量下,大部分农药秋季的原始沉积量、最大残留量大于夏季的原始沉积量和最大残留量。在相同的收获间隔期时,石家庄样品中超过85%农药秋季的残留量高于夏季残留量,北京样品几乎所有农药残留量均高于夏季残留量。为验证以上试验结果,对嘧菌酯、精吡氟禾草灵、噻嗪酮、杀扑磷、噻虫嗪、腐霉利和高效氯氰菊酯在石家庄、北京和南京进行一年两季的残留试验。试验结果表明,在相同的施药剂量下大部分农药秋季原始沉积量、最大残留量高于夏季的原始沉积量和最大残留量；超过70%样品中农药秋季的残留量高于夏季残留量。方差分析结果表明不同生长季节对农药原始沉积量和半衰期的影响较大,对最终残留量影响较小。
为考察不同施药次数对农药残留规律的影响,对嘧菌酯、精吡氟禾草灵、噻嗪酮、杀扑磷、噻虫嗪、腐霉利和高效氯氰菊酯在芹菜上进行一年两季(夏季和秋季)的残留实验,试验设计施药一次和两次,从农药消解动态、原始沉积量、最大残留量、最终残留量等几个方面考察不同施药次数对农药残留行为的影响。结果表明,施药间隔7d时,夏季试验时约64%的农药施药两次时半衰期比施药一次时半衰期长,秋季试验时越50%的农药施药两次时半衰期比施药一次时半衰期长。石家庄夏季试验结果表明,芹菜施药两次时嘧菌酯、噻嗪酮、杀扑磷、噻虫嗪和高效氯氰菊酯的原始沉积量比施药一次时高；秋季试验施药两次时7种农药的原始沉积量均比施药一次要高,而且原始沉积量增加的幅度比夏季试验时要高很多,特别是嘧菌酯和高效氯氰菊酯。北京的试验结果跟石家庄一致,施药两次时农药的原始沉积量比施药一次时高(夏季试验嘧菌酯除外),而且秋季试验时原始沉积量增长比例比夏季施药时要高。夏季试验时约60%的农药施药两次时,最终残留量较施药一次有升高；而同样的施药剂量条件下秋季试验时超过90%的农药施药两次时,农药的最终残留量比施药一次时残留量更高。方差分析结果表明不同施药次数时芹菜中农药的原始沉积量、半衰期和最终残留量均无显著差异。
对六种绿叶蔬菜中农药残留进行了膳食摄入风险评估。从多菌灵等5种农药慢性风险评估结果来看,菠菜和苋菜或叶用莴苣的慢性风险较高；从嘧菌酯等7种农药慢性风险评估结果来看,菠菜和苋菜或茼蒿的慢性风险较高。多菌灵等5种农药急性风险评估结果表明菠菜和苋菜中急性风险比较高,嘧菌酯等7种农药急性风险评估结果也表明菠菜和苋菜中急性风险较高。膳食摄入风险评估综合了农药田间试验残留数据和食物的摄入水平,从风险评估结果来看,菠菜或苋菜可作为绿叶蔬菜的代表作物。
Ilegal usage, incorrect usage of pesticides, pesticides application out of the label, and the lack of maximum residue limits are the core issues of agricultural products and food safety. Crops are classified and grouped accourding to their morphology and residue characteristics, representative commodities are chosen based on their commercial importance and the similarity of their morphology and residue characteristics to other related commodities in the group or suboup. Supervised field residue trials of representative commodities will be conducted according to good agriculture production, and the residues datas could be used in the residue extrapolation, which is a scientific and effective solution to resolve relative problems such as lack of pesticide registration on minor crop and the absence of maximum residue limits.
In this study, a multi-residue method was built to determine of thiophanate-methyl, carbendazim, metalaxyl, fluazifop-P-butyl, azoxystrobin, buprofezin, methidathion, thiamethoxam, procymidone, chlorpyrifos, lambda-cyhalothrin, beta-cypermethrin in pakchoi, rape, crown daisy, amaranth, spinach, lettuce and celery. A quick, easy, cheap, effective, rugged and safe (QuEChERS) method was used in*sample preparation, thiophanate-methyl, carbendazim, metalaxyl, fluazifop-P-butyl, azoxystrobin, buprofezin, methidathion, thiamethoxam and procymidone were detected by liquid chromatography tandem mass spectrometry (LC-MS/MS), chlorpyrifos, lambda-cyhalothrin and beta-cypermethrin were determined by gas chromatography with electron capture detector (GC-ECD). The limits of quantification (LOQ) in all leafy vegetables were in the range of0.001-0.08mg/kg for all analytes and the average recoveries of all pesticides ranged from60.1%to118.6%. Good linearity was found for all pesticides with cofficients between0.991and1.00in a range of0.001-10.0mg/kg. The developed method was successfully used to determine the12pesticide residues in seven leafy vegetables.
To select representative commodities in leafy green vegetables and for adorption in establishment of maximum residue limits of pesticides, supervised field residue trails of thiophanate-methyl, fluazifop-P-butyl, metalaxyl, chlorpyrifos and lambda-cyhalothrin on six leafy green vegetables including pakchoi, rape, crown daisy, amaranth, spinach and lettuce were designed and conducted in three places. It was found that almost all initial concentrations and maximal concentrations of pesticides in spinach and/or amaranth were higher than others with the same application dose, and the final residues for most pesticides in shinach and/or amaranth at the same preharvest interval (PHI) were higher. Spinach and/or amaranth were selected as representative crop in leafy green vegetables. In order to verify the accuracy of representative commodities selected, supervised field residue trials of azoxystrobin, fluazifop-P-butyl, buprofezin, methidathion, thiamethoxam, procymidone, beta-cypermethrin in the six leaf vegetables were conducted in three places. Initial concentrations, maximal concentrations and final residues were also used to compare. In addition to the part of higher final residues in crown daisy, the other results were consistent. In consideration of residue dynamics, initial concentrations and final residues, spinach and/or amaranth were recommended to select as representative commodities in leafy green vegetables.
To investigate the influence of different planting seasons on the dissipation of pesticides, supervised field residue trails of thiophanate-methyl, metalaxyl, fluazifop-P-butyl, chlorpyrifos and lambda-cyhalothrin on six leafy green vegetables including pakchoi, rape, crown daisy, amaranth, spinach and lettuce were designed and conducted at two planting seasons (summer:between May and July; autumn:between August and October) in three places. The results showed that initial concentrations and maximal concentrations of most pesticides in six leafy green vegetables at autumn were higher that at summer. More than85%samples contained more pesticide residues at autumn at the same PHI in Shijiazhuang, and almost all samples had higher concentrations of pesticides at autumn at same PHI in Beijing. In order to verify the conclusion above, supervised field residue trails of azoxystrobin, fluazifop-P-butyl, buprofezin, methidathion, thiamethoxam, procymidone, beta-cypermethrin in the six leafy green vegetables were conducted at two planting seasons in Shijiazhuang, Beijing and Nanjing. For most pesticides, the initial concentrations and maximal concentrations at autumn were higher than that at summer with the same spray dose More than70%samples contained more pesticide residues at autumn at the same PHI. Analysis variance results showed that initial concentrations and half-lives of pesticides were influced by different planting seasons in a larger degree than the final residues.
In order to investigate the effect of different spraying times on pesticide residues, supervised field residue trails of azoxystrobin, fluazifop-P-butyl, buprofezin, methidathion, thiamethoxam, procymidone, beta-cypermethrin in celery were conducted at two planting seasons. The experiments were designed for spraying one time and two times. Initial concentrantions, maximal concentrations and final concentrations of pesticides were considered in data analysis. The results of the experiments showed that half-lives of about64%pesticides were longer when sprayed two times (spraying pesticide interval was7days) than that sprayed one time at summer, and half-lives of about50%pesticides were longer when sprayed two times at autumn. The initial concentrations of azoxystrobin, buprofezin, methidathion, thiamethoxam, beta-cypermethrin in celery when spraying two times were higher than that when spraying one time at summer in Shijiazhuang, the initial concentrations of the seven pesticides when spraying two times were higher than that spraying one time at autumn, and the increase was higher at autumn especially to azoxystrobin and beta-cypermethrin. The results of Beijing were consistent with that of Shijiazhuang, initial concentrations of pesticides when spraying two times were higher than that when spraying one time in Beijing in addition to the azoxystrobin at summer. Approximately60%samples contained more pesticide residues when spraying two times at summer, while more than90%samples had higher concentrations of pesticides when spraying two times at autumn. There were no significant differences in initial concentrations, half-lives and final residues in celery with different spraying times.
The dietary risk assessment of pesticides in six leafy green vegetables was conducted. The chronic assessment results of five pestides (carbendazim etc.) demonstrated that chronic dietary risk of spinach and amaranth (or leaf lettuce) was much higher; and the chronic assessment results of seven pesticides (azoxystrobin etc.) indicated that chronic dietary risk of spinach and amaranth (or crown daisy) was much higher. The acute assessment results of five pestides (carbendazim etc.) showed that acute dietary risk of spinach and/or amaranth was higher; and acute assessment results of seven pesticides (azoxystrobin etc.) presented that the acute dietary risk of spinach and/or amaranth was higher. Risk assessment is a comprehensive indicator in that it reflects the field experiment results and the dietary intake at same time. Spinach and/or amaranth could be recommended to select as representative commodities in according to the risk assessment results.
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