水果中农药残留分析方法研究
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摘要
本论文研究内容有两部分。第一部分为水果中克菌丹和灭菌丹残留分析方法研究;第二部分为苹果中醚菌酯、戊唑醇和苯醚甲环唑残留分析方法研究。
通过研究我们获得了如下成果:
(1)建立了以乙腈提取,硅镁吸附剂+硅胶净化,正己烷+二氯甲烷+乙腈(50+49+1)混合溶剂洗脱,用电子捕获检测器气相色谱法测定水果中克菌丹和灭菌丹的残留量的分析方法。研究了洗脱溶剂及洗脱溶剂的体积、固相萃取柱、pH值和加水量以及吸附剂的稳定性等影响因素对克菌丹和灭菌丹测定的影响。在0.05mg/L～2.00mg/L的浓度范围内,克菌丹和灭菌丹的含量与峰面积成线性关系,相关系数均大于0.997;对苹果、波萝、草莓、梨和橙子5种水果进行分析,克菌丹和灭菌丹三个浓度水平的回收率分别在89.3%～115%和77.5%～117%之间;相对标准偏差范围分别在2.5%～7.5%和2.8%～8.0%之间。方法的检出限分别为0.012mg/kg和0.006mg/kg,所建立的分析方法准确度高,重现性好。
(2)建立了以乙腈提取,硅镁吸附剂+硅胶净化,正己烷+二氯甲烷+乙腈(50+49+1)混合溶剂洗脱,以紫外检测器液相色谱法测定苹果中的克菌丹和灭菌丹残留量的分析方法。详细研究了色谱柱、流动相以及检测波长对克菌丹和灭菌丹测定的影响;并比较了不同固相萃取柱和不同洗脱溶剂测定克菌丹和灭菌丹的结果。以Eclipse XDB-C18为分离柱,甲醇-乙腈-水(内含0.1mmol/L,pH=3.80的乙酸-乙酸钠缓冲溶液)(50+5+45)为流动相,测定波长选为210nm,在10.00～200.00mg/L浓度范围内,克菌丹和灭菌丹的含量与峰面积成线性关系,相关系数均大于0.9999,克菌丹和灭菌丹三个浓度水平的回收率范围分别在63.9%～111%和101%～110%之间,相对标准偏差分别在2.5%～4.8%和1.4%～2.3%之间。所建立的分析方法测定克菌丹和灭菌丹的重现性好,方法准确可靠,适合克菌丹和灭菌丹残留量比较高的样品测定。通过气相色谱法与液相色谱法的比对得出,气相色谱法比液相色谱法准确度高,精密度好,灵敏度高。
(3)建立了以乙腈提取,NH2柱净化,丙酮+正己烷(50+50)混合溶剂洗脱,电子捕获检测器气相色谱法测定苹果中醚菌酯、戊唑醇和苯醚甲环唑的残留量的分析方法。研究了提取溶剂、洗脱溶剂及洗脱溶剂的体积、固相萃取柱和加水量等影响因素对醚菌酯、戊唑醇和苯醚甲环唑测定的影响。在所测定的浓度范围内,醚菌酯、戊唑醇和苯醚甲环唑的含量与峰面积成线性关系,相关系数均大于0.99。对苹果进行实际样品分析,醚菌酯、戊唑醇和苯醚甲环唑三个浓度水平的平均回收率分别在110% ~ 115%、105% ~ 112%和81.6% ~ 112%之间;相对标准偏差分别在1.7% ~5.9%、2.1% ~ 9.8%和4.3% ~9.5%之间,方法准确度高,精密度好。
本文建立的水果中克菌丹灭菌丹残留量的标准分析方法,其检出限能够达到mg/kg级(或μg/kg级),并且能够同时测定水果以及蔬菜中克菌丹和灭菌丹的残留量,该方法操作简单,结果准确,费用低,适合国情。建立的苹果中醚菌酯、戊唑醇和苯醚甲环唑残留量的标准分析方法,其检出限能够达到mg/kg级甚至μg/kg级,并且能够同时测定苹果中醚菌酯、戊唑醇和苯醚甲环唑的残留量,方法操作简单、快速,结果准确。在国内没有检验标准的情况下,为同时测定水果中的醚菌酯、戊唑醇和苯醚甲环唑提供参考方法。
The achievements of the study were as follows:
(1) An analytical method was developed on the simultaneous determination of captan and folpet in fruits by SPE-GC-ECD. The sample was extracted with acetonitrile, cleaned by SPE with silica magnesium sorbent+silica gel, with hexane-dichloromethane-acetonitrile (50+49+1) as eluent. The influencing factors including eluting solvent and its volume, SPE column, pH, volume of water added and stability of the sorbent were discussed. In the concentration range from 0.05mg/L to 2.00mg/L, captan and folpet both had good linearity. Recoveries from spiked samples ranged from 81.5% to 116% and RSDs were not higher than 8.0%.
(2) An analytical method was developed on the determination of captan and folpet in apples by SPE-HPLC-UV. The steps for pesticides residues extraction and purification were similar with that in ChapterⅡ. The mobile phase is a mixture of methanol, acetonitrile and water (0.1mmol/L buffer of acetic acid - ammonium acetate)(50+5+45) at the flow rate of 1.0mL/min. The separation was carried out using an Eclipse XDB-C18 column and UV was set at 210nm. In the concentration range from 10.00mg/L to 200.00mg /L, captan and folpet both had good linearity. Recoveries from spiked samples ranged from 63.9% to 111% and relative standard deviations were not higher than 4.8%. Limits of detection were 0.68mg/kg and 0.50mg/kg for captan and folpet, respectively. The method is precise and accurate for high concentration of captan and folpet, it is suitable for determining of high concentration of captan and folpet in apples. The method of high performance liquid chromatography was compared with gas chromatography through accuracy, precision and sensitivity. It showed that gas chromatography was more accurate, precise and sensitive than high performance liquid chromatography.
(3) An analytical method was developed on the determination of kresoxim-methyl, tebuconazole and difenoconazole in apples by SPE-GC-ECD. The sample was extracted with acetonitrile, cleaned by solid phase extraction with NH2, eluted with acetone-hexane (50+50). The influencing factors including eluting solvent and its volume, SPE column and volume of water added were discussed. In the concentration range we determined, kresoxim-methyl, tebuconazole and difenoconazole all had good linearity. Recoveries from spiked samples ranged from 81.6% to 115%; and RSDs were not higher than 10%.
The method for simutaneous determination of captan and folpet in fruits, it can determine captan and folpet at the same time, and it was simple, accurate, cheap, so it was suitable for our country. The method for simutaneous determination of kresoxim-methyl, tebuconazole and difenoconazole in apples, it was simple, accurate; and in the case of there were no standard methods for kresoxim-methyl, tebuconazole and difenoconazole in China, it provided reference method for the determination of them in apples.
通过研究我们获得了如下成果:
(1)建立了以乙腈提取,硅镁吸附剂+硅胶净化,正己烷+二氯甲烷+乙腈(50+49+1)混合溶剂洗脱,用电子捕获检测器气相色谱法测定水果中克菌丹和灭菌丹的残留量的分析方法。研究了洗脱溶剂及洗脱溶剂的体积、固相萃取柱、pH值和加水量以及吸附剂的稳定性等影响因素对克菌丹和灭菌丹测定的影响。在0.05mg/L～2.00mg/L的浓度范围内,克菌丹和灭菌丹的含量与峰面积成线性关系,相关系数均大于0.997;对苹果、波萝、草莓、梨和橙子5种水果进行分析,克菌丹和灭菌丹三个浓度水平的回收率分别在89.3%～115%和77.5%～117%之间;相对标准偏差范围分别在2.5%～7.5%和2.8%～8.0%之间。方法的检出限分别为0.012mg/kg和0.006mg/kg,所建立的分析方法准确度高,重现性好。
(2)建立了以乙腈提取,硅镁吸附剂+硅胶净化,正己烷+二氯甲烷+乙腈(50+49+1)混合溶剂洗脱,以紫外检测器液相色谱法测定苹果中的克菌丹和灭菌丹残留量的分析方法。详细研究了色谱柱、流动相以及检测波长对克菌丹和灭菌丹测定的影响;并比较了不同固相萃取柱和不同洗脱溶剂测定克菌丹和灭菌丹的结果。以Eclipse XDB-C18为分离柱,甲醇-乙腈-水(内含0.1mmol/L,pH=3.80的乙酸-乙酸钠缓冲溶液)(50+5+45)为流动相,测定波长选为210nm,在10.00～200.00mg/L浓度范围内,克菌丹和灭菌丹的含量与峰面积成线性关系,相关系数均大于0.9999,克菌丹和灭菌丹三个浓度水平的回收率范围分别在63.9%～111%和101%～110%之间,相对标准偏差分别在2.5%～4.8%和1.4%～2.3%之间。所建立的分析方法测定克菌丹和灭菌丹的重现性好,方法准确可靠,适合克菌丹和灭菌丹残留量比较高的样品测定。通过气相色谱法与液相色谱法的比对得出,气相色谱法比液相色谱法准确度高,精密度好,灵敏度高。
(3)建立了以乙腈提取,NH2柱净化,丙酮+正己烷(50+50)混合溶剂洗脱,电子捕获检测器气相色谱法测定苹果中醚菌酯、戊唑醇和苯醚甲环唑的残留量的分析方法。研究了提取溶剂、洗脱溶剂及洗脱溶剂的体积、固相萃取柱和加水量等影响因素对醚菌酯、戊唑醇和苯醚甲环唑测定的影响。在所测定的浓度范围内,醚菌酯、戊唑醇和苯醚甲环唑的含量与峰面积成线性关系,相关系数均大于0.99。对苹果进行实际样品分析,醚菌酯、戊唑醇和苯醚甲环唑三个浓度水平的平均回收率分别在110% ~ 115%、105% ~ 112%和81.6% ~ 112%之间;相对标准偏差分别在1.7% ~5.9%、2.1% ~ 9.8%和4.3% ~9.5%之间,方法准确度高,精密度好。
本文建立的水果中克菌丹灭菌丹残留量的标准分析方法,其检出限能够达到mg/kg级(或μg/kg级),并且能够同时测定水果以及蔬菜中克菌丹和灭菌丹的残留量,该方法操作简单,结果准确,费用低,适合国情。建立的苹果中醚菌酯、戊唑醇和苯醚甲环唑残留量的标准分析方法,其检出限能够达到mg/kg级甚至μg/kg级,并且能够同时测定苹果中醚菌酯、戊唑醇和苯醚甲环唑的残留量,方法操作简单、快速,结果准确。在国内没有检验标准的情况下,为同时测定水果中的醚菌酯、戊唑醇和苯醚甲环唑提供参考方法。
The achievements of the study were as follows:
(1) An analytical method was developed on the simultaneous determination of captan and folpet in fruits by SPE-GC-ECD. The sample was extracted with acetonitrile, cleaned by SPE with silica magnesium sorbent+silica gel, with hexane-dichloromethane-acetonitrile (50+49+1) as eluent. The influencing factors including eluting solvent and its volume, SPE column, pH, volume of water added and stability of the sorbent were discussed. In the concentration range from 0.05mg/L to 2.00mg/L, captan and folpet both had good linearity. Recoveries from spiked samples ranged from 81.5% to 116% and RSDs were not higher than 8.0%.
(2) An analytical method was developed on the determination of captan and folpet in apples by SPE-HPLC-UV. The steps for pesticides residues extraction and purification were similar with that in ChapterⅡ. The mobile phase is a mixture of methanol, acetonitrile and water (0.1mmol/L buffer of acetic acid - ammonium acetate)(50+5+45) at the flow rate of 1.0mL/min. The separation was carried out using an Eclipse XDB-C18 column and UV was set at 210nm. In the concentration range from 10.00mg/L to 200.00mg /L, captan and folpet both had good linearity. Recoveries from spiked samples ranged from 63.9% to 111% and relative standard deviations were not higher than 4.8%. Limits of detection were 0.68mg/kg and 0.50mg/kg for captan and folpet, respectively. The method is precise and accurate for high concentration of captan and folpet, it is suitable for determining of high concentration of captan and folpet in apples. The method of high performance liquid chromatography was compared with gas chromatography through accuracy, precision and sensitivity. It showed that gas chromatography was more accurate, precise and sensitive than high performance liquid chromatography.
(3) An analytical method was developed on the determination of kresoxim-methyl, tebuconazole and difenoconazole in apples by SPE-GC-ECD. The sample was extracted with acetonitrile, cleaned by solid phase extraction with NH2, eluted with acetone-hexane (50+50). The influencing factors including eluting solvent and its volume, SPE column and volume of water added were discussed. In the concentration range we determined, kresoxim-methyl, tebuconazole and difenoconazole all had good linearity. Recoveries from spiked samples ranged from 81.6% to 115%; and RSDs were not higher than 10%.
The method for simutaneous determination of captan and folpet in fruits, it can determine captan and folpet at the same time, and it was simple, accurate, cheap, so it was suitable for our country. The method for simutaneous determination of kresoxim-methyl, tebuconazole and difenoconazole in apples, it was simple, accurate; and in the case of there were no standard methods for kresoxim-methyl, tebuconazole and difenoconazole in China, it provided reference method for the determination of them in apples.
引文
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