毛细管电泳富集新技术在农药残留及药物分析中的应用
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摘要
毛细管电泳(Capillary Electrophoresis, CE)以其分离效率高、分析时间短、样品需要量少、操作费用低等优点,日益成为一种高效的分离分析方法。但由于其进样体积小和检测光程短,对常用的紫外检测器而言,CE的一个主要缺陷是灵敏度较低,解决此问题的一个有效途径是采用离线或在线样品富集的方法。在线富集技术具有简单经济,无需对商品仪器进行改造的优点。样品在线富集方法如推扫、阴阳离子耗尽进样一推扫、场放大样品堆积、pH调制酸(碱)堆积、pH梯度一推扫、胶束解离样品堆积、胶束有机溶剂堆积等己经成功应用于各种样品的分析中。在系统查阅有关文献资料的基础上,进行了以下研究工作:
1.建立了分散液液微萃取与胶束毛细管电动色谱在线推扫(DLLME-sweeping- MEKC)测水样中的三嗪类除草剂残留的快速、灵敏检测方法。并对影响萃取和推扫效果的参数,例如萃取剂和分散剂的种类及用量、萃取时间、加盐量、水溶液pH值、缓冲溶液pH、浓度进行了优化。在最优条件下,五类除草剂的富集倍率高达17540~28 800。此方法的线性获得范围0.15~20 ng/mL,线性相关系数范围为0.9994~0.9997,检出限为0.05~0.10 ng/mL。日内相对标准偏差为1.5%~5.1% (n=5)和2.9%~5.6%(n =15)。在河水、井水和地表水水样中五类除草剂相对回收率在0.5 ng/mL和20.0 ng/mL的混合水平上分别为94.9%~112.0%和80.7%~100.6%。该方法已成功地应用于分析实际水样中的三嗪类除草剂残留。
2.建立了分散液液微萃取与胶束毛细管电动色谱在线推扫测定黄瓜中的烟碱类杀虫剂(噻虫啉、啶虫脒、氯噻啉和吡虫啉)残留的快速、灵敏的新方法。并对影响萃取和推扫效果的因素、萃取剂和分散剂的种类及用量、萃取时间、盐浓度、样品基质和缓冲溶液浓度等进行了优化。在最优条件下,此方法的富集倍率达到4320~9957倍(峰面积),检出限为0.7~1.2 ng/g,定量限(信噪比为10:1)3~5 ng/g,线性范围噻虫嗪,啶虫脒和吡虫啉为4.0~200 ng/g,氯噻啉为5.0~200 ng/g。日内和日间相对标准偏差范围分别是3.8%~4.4%(n=5)和6.5%~8.5%(n=15)。在黄瓜中加标浓度为10 ng/g和50 ng/g的相对回收率在83.0%~98.6%之间,相对标准偏差低于6.3%。该方法已成功地应用于分析黄瓜样品中的烟碱类杀虫剂。
3.建立了胶束溶剂堆积毛细管区带电泳法(MSS-CZE)测定马钱子制剂中的士宁和马钱子碱的含量。选择pH 4.0 30 mmol/L磷酸盐(含20%乙腈)为缓冲液,样品基质:8 mmol/L磷酸盐,5 mmol /LSDS为样品基质;分离电压20 kV,进样0.5 psi 150s,DAD检测波203 nm。士的宁和马钱子碱的浓度在0.2~15.0μg/mL内线性良好,线性相关系数分别为0. 9984和0. 9976,在中药制剂样品中加标回收率均在94.1%~114.4%之间,检测限分别0.02和0.05μg/mL。相对标准偏差在2.21%~4.56%之间MSS-CZE可有效地分离、测定马钱子中药制剂中的士的宁和马钱子碱的含量,方法简便、快速、准确、可靠。可作为药材中有效成分质量控制的方法。
4.建立了胶束解离样品富集胶束毛细管电动色谱方法(AFMC-MEKC)测定苦参及其制剂中的氧化苦参碱和苦参碱的方法。选择20 mmol/LpH 9.5硼砂和30 mmol/L SDS(含30%甲醇)为缓冲液,6 mmol/LSDS,30 mmol/L硼砂为样品基质,未涂层熔融石英毛细管柱(内径75μm,总长50 cm,有效长度40 cm)分离电压20 kV,进样0.5 psi,120 s,紫外检测波长205 nm,温度25℃的条件下进行测定。氧化苦参碱,苦参碱的浓度在1.0~100.0μg/mL范围内与峰面积呈良好的线性关系,线性相关系数分别为0.9954和0.9996,检出限分别为0.3,0.02μg/mL。该方法已用于苦参及其苦参片制剂药品中氧化苦参碱和苦参碱含量的测定,其样品平均回收率在96.3%~107.2 %之间,取得了满意的结果。
Capillary electrophoresis (CE) has been recognized as a highly attractive separation technique due to its high separation efficiency, short analysis time, small sample requirements and low operation cost. However, the main drawback of CE is the poor concentration sensitivity due to the small injection volumes and a short optical path length in the most commonly used UV detection. One solution to the problem is to apply off-line and/ or on-line sample concentration methods. The on-line concentration techniques have advantages of simplicity and economy because of no requirements of modification in CE instrumentation. Some on-line concentration techniques such as sweeping, anion or cation selective exhaustive injection-sweeping, large volume sample stacking, field-enhanced sample stacking, acid or base pH-mediated stacking dynamic pH junction-sweeping, micelle to solvent stacking and analyte focusing by micelle collapse have enjoyed much success to the analysis of many types of samples. This thesis is mainly concerned with the following aspects:
1. A rapid, sensitive method for the multiresidue analysis of five commonly used triazine herbicides in environment waters was developed using dispersive liquid–liquid microextraction (DLLME) coupled with on-line sweeping in micellar electrokinetic chromatography (MEKC). Parameters that affect the extraction and sweeping efficiency, such as the kind and volume of the extraction and disperser solvent, extraction time, salt addition, the pH in water sample, the pH and concentration of separation buffer were investigated and optimized. Under the optimum conditions, the enrichment factors were achieved in the range of 17540 to 28800. The linearity of the method was obtained in the range of 0.15~20 ng/mL with the correlation coefficients (r2) ranging from 0.9994 to 0.9997. The limits of detection were 0.05~0.1 ng/mL. The intraday relative standard deviations (RSDs) varied from 1.5 % to 5.1 % (n=5) and interday from 2.9% to 5.6% (n =15). The relative recoveries of the five herbicides in water samples at spiking levels of 0.5 ng/mL and 15 ng/mL were 94.9%~112.0% and 80.7%~100.6%. The proposed method has been successfully applied to the analysis of target herbicide residues in water samples with satisfactory results.
2. A novel method was developed by using dispersive liquid–liquid microextraction (DLLME) coupled with sweeping-MEKC for the multiresidue analysis of chloronicotinyl insecticide thiacloprid (TCL),acetamiprid (ACT), imidaclothiz(ICZ) and imidacloprid (ICL) in cucumbers. Parameters that affect the extraction and sweeping efficiency, such as the kind and volume of the extraction and disperser solvent, extraction time and salt addition, sample matrix and organic modifiers concentration in separation buffer were investigated and optimized. Under the optimum conditions, the enrichment factors were achieved in the range of 4320~9957 (EFA). The linearity of the method for thiacloprid, acetamiprid, and imidacloprid was in the range of 4.0- 200 ng/g in cucumber samples, and for imidaclothiz ranged from 5.0 to 200 ng/g, with the correlation coefficients (r) ranging from 0.9961 to 0.9984, respectively. The limits of detection (LODs, S/N=3) ranged from 0.7 to 1.2 ng/g. The intraday relative standard deviations (RSDs) varied from 3.8% to 4.4% (n=5) and interday from 6.5% to 8.5% (n =15). The recoveries in cucumbers at spiking levels of 10 ng/g and 100 ng/g were ranging from 83.0 to 98.6% with the RSDs lower than 6.3%. The proposed method has been successfully applied to the analysis of target chloronicotinyl insecticide residues in cucumber samples with satisfactory results.
3. The determination of strychnine and brucine in traditional Chinese medicine preparation was established by micelle to solvent stacking in capillary zone electrophoresis. The optimal condition of the running buffer solution was 30 mmol/L phosphates containing 20% acetonitrile at pH 4.00. The sample matrix was 8 mmol/L phosphate and 5 mmol/L SDS pH 3.00. The samples were injected with pressure at 0.5 psi for 150 s. The applied voltage was 20 kV and the wavelength of the detection was 205 nm.The method had good linearity and reproducibility in the range of strychnine and brucine, the correlation coefficients (r) were 0.9984~0.9976. The relative recoveries of strychnine and brucine in Traditional Chinese medicine were 94.1%~114.4%. In this condition, strychnine and brucine can be well separated from the other components. The method is convenient, rapid, accurate and reliable, and can be used to control the quality of effective components in Traditional Chinese medicine.
4. A novel method for the determination of oxymatrin and matrin in Sophora flavescens Ait. and Chinese medicine preparation by analyte focusing by micelle collapse in micellar electrokinetic chromatography. The optimal condition of the running buffer solution was 20 mmol/L sodium borate, 30 mmol /L SDS and 25% methanol at pH 9.50. The sample matrix was 30 mmol/L sodium borate and 6 mmol/L SDS. The samples were injected with pressure at 0.5 psi for 120s. The applied voltage was 20 kV and the wavelength of the detection was 205 nm.The calibration curve was linear over a range of 0.5~10μg/mL for oxymatrin and matrin, with correlation coefficients of 0.992and 0.993, respectively. The detection limits (S/N = 3:1)for oxymatrin and matrin were 0.10 and 0.20μg/ml, respectively. The relative recoveries of oxymatrin and matrin in Traditional Chinese medicine and Sophora flavescens Ait. were 94.1%~114.4%.
1.建立了分散液液微萃取与胶束毛细管电动色谱在线推扫(DLLME-sweeping- MEKC)测水样中的三嗪类除草剂残留的快速、灵敏检测方法。并对影响萃取和推扫效果的参数,例如萃取剂和分散剂的种类及用量、萃取时间、加盐量、水溶液pH值、缓冲溶液pH、浓度进行了优化。在最优条件下,五类除草剂的富集倍率高达17540~28 800。此方法的线性获得范围0.15~20 ng/mL,线性相关系数范围为0.9994~0.9997,检出限为0.05~0.10 ng/mL。日内相对标准偏差为1.5%~5.1% (n=5)和2.9%~5.6%(n =15)。在河水、井水和地表水水样中五类除草剂相对回收率在0.5 ng/mL和20.0 ng/mL的混合水平上分别为94.9%~112.0%和80.7%~100.6%。该方法已成功地应用于分析实际水样中的三嗪类除草剂残留。
2.建立了分散液液微萃取与胶束毛细管电动色谱在线推扫测定黄瓜中的烟碱类杀虫剂(噻虫啉、啶虫脒、氯噻啉和吡虫啉)残留的快速、灵敏的新方法。并对影响萃取和推扫效果的因素、萃取剂和分散剂的种类及用量、萃取时间、盐浓度、样品基质和缓冲溶液浓度等进行了优化。在最优条件下,此方法的富集倍率达到4320~9957倍(峰面积),检出限为0.7~1.2 ng/g,定量限(信噪比为10:1)3~5 ng/g,线性范围噻虫嗪,啶虫脒和吡虫啉为4.0~200 ng/g,氯噻啉为5.0~200 ng/g。日内和日间相对标准偏差范围分别是3.8%~4.4%(n=5)和6.5%~8.5%(n=15)。在黄瓜中加标浓度为10 ng/g和50 ng/g的相对回收率在83.0%~98.6%之间,相对标准偏差低于6.3%。该方法已成功地应用于分析黄瓜样品中的烟碱类杀虫剂。
3.建立了胶束溶剂堆积毛细管区带电泳法(MSS-CZE)测定马钱子制剂中的士宁和马钱子碱的含量。选择pH 4.0 30 mmol/L磷酸盐(含20%乙腈)为缓冲液,样品基质:8 mmol/L磷酸盐,5 mmol /LSDS为样品基质;分离电压20 kV,进样0.5 psi 150s,DAD检测波203 nm。士的宁和马钱子碱的浓度在0.2~15.0μg/mL内线性良好,线性相关系数分别为0. 9984和0. 9976,在中药制剂样品中加标回收率均在94.1%~114.4%之间,检测限分别0.02和0.05μg/mL。相对标准偏差在2.21%~4.56%之间MSS-CZE可有效地分离、测定马钱子中药制剂中的士的宁和马钱子碱的含量,方法简便、快速、准确、可靠。可作为药材中有效成分质量控制的方法。
4.建立了胶束解离样品富集胶束毛细管电动色谱方法(AFMC-MEKC)测定苦参及其制剂中的氧化苦参碱和苦参碱的方法。选择20 mmol/LpH 9.5硼砂和30 mmol/L SDS(含30%甲醇)为缓冲液,6 mmol/LSDS,30 mmol/L硼砂为样品基质,未涂层熔融石英毛细管柱(内径75μm,总长50 cm,有效长度40 cm)分离电压20 kV,进样0.5 psi,120 s,紫外检测波长205 nm,温度25℃的条件下进行测定。氧化苦参碱,苦参碱的浓度在1.0~100.0μg/mL范围内与峰面积呈良好的线性关系,线性相关系数分别为0.9954和0.9996,检出限分别为0.3,0.02μg/mL。该方法已用于苦参及其苦参片制剂药品中氧化苦参碱和苦参碱含量的测定,其样品平均回收率在96.3%~107.2 %之间,取得了满意的结果。
Capillary electrophoresis (CE) has been recognized as a highly attractive separation technique due to its high separation efficiency, short analysis time, small sample requirements and low operation cost. However, the main drawback of CE is the poor concentration sensitivity due to the small injection volumes and a short optical path length in the most commonly used UV detection. One solution to the problem is to apply off-line and/ or on-line sample concentration methods. The on-line concentration techniques have advantages of simplicity and economy because of no requirements of modification in CE instrumentation. Some on-line concentration techniques such as sweeping, anion or cation selective exhaustive injection-sweeping, large volume sample stacking, field-enhanced sample stacking, acid or base pH-mediated stacking dynamic pH junction-sweeping, micelle to solvent stacking and analyte focusing by micelle collapse have enjoyed much success to the analysis of many types of samples. This thesis is mainly concerned with the following aspects:
1. A rapid, sensitive method for the multiresidue analysis of five commonly used triazine herbicides in environment waters was developed using dispersive liquid–liquid microextraction (DLLME) coupled with on-line sweeping in micellar electrokinetic chromatography (MEKC). Parameters that affect the extraction and sweeping efficiency, such as the kind and volume of the extraction and disperser solvent, extraction time, salt addition, the pH in water sample, the pH and concentration of separation buffer were investigated and optimized. Under the optimum conditions, the enrichment factors were achieved in the range of 17540 to 28800. The linearity of the method was obtained in the range of 0.15~20 ng/mL with the correlation coefficients (r2) ranging from 0.9994 to 0.9997. The limits of detection were 0.05~0.1 ng/mL. The intraday relative standard deviations (RSDs) varied from 1.5 % to 5.1 % (n=5) and interday from 2.9% to 5.6% (n =15). The relative recoveries of the five herbicides in water samples at spiking levels of 0.5 ng/mL and 15 ng/mL were 94.9%~112.0% and 80.7%~100.6%. The proposed method has been successfully applied to the analysis of target herbicide residues in water samples with satisfactory results.
2. A novel method was developed by using dispersive liquid–liquid microextraction (DLLME) coupled with sweeping-MEKC for the multiresidue analysis of chloronicotinyl insecticide thiacloprid (TCL),acetamiprid (ACT), imidaclothiz(ICZ) and imidacloprid (ICL) in cucumbers. Parameters that affect the extraction and sweeping efficiency, such as the kind and volume of the extraction and disperser solvent, extraction time and salt addition, sample matrix and organic modifiers concentration in separation buffer were investigated and optimized. Under the optimum conditions, the enrichment factors were achieved in the range of 4320~9957 (EFA). The linearity of the method for thiacloprid, acetamiprid, and imidacloprid was in the range of 4.0- 200 ng/g in cucumber samples, and for imidaclothiz ranged from 5.0 to 200 ng/g, with the correlation coefficients (r) ranging from 0.9961 to 0.9984, respectively. The limits of detection (LODs, S/N=3) ranged from 0.7 to 1.2 ng/g. The intraday relative standard deviations (RSDs) varied from 3.8% to 4.4% (n=5) and interday from 6.5% to 8.5% (n =15). The recoveries in cucumbers at spiking levels of 10 ng/g and 100 ng/g were ranging from 83.0 to 98.6% with the RSDs lower than 6.3%. The proposed method has been successfully applied to the analysis of target chloronicotinyl insecticide residues in cucumber samples with satisfactory results.
3. The determination of strychnine and brucine in traditional Chinese medicine preparation was established by micelle to solvent stacking in capillary zone electrophoresis. The optimal condition of the running buffer solution was 30 mmol/L phosphates containing 20% acetonitrile at pH 4.00. The sample matrix was 8 mmol/L phosphate and 5 mmol/L SDS pH 3.00. The samples were injected with pressure at 0.5 psi for 150 s. The applied voltage was 20 kV and the wavelength of the detection was 205 nm.The method had good linearity and reproducibility in the range of strychnine and brucine, the correlation coefficients (r) were 0.9984~0.9976. The relative recoveries of strychnine and brucine in Traditional Chinese medicine were 94.1%~114.4%. In this condition, strychnine and brucine can be well separated from the other components. The method is convenient, rapid, accurate and reliable, and can be used to control the quality of effective components in Traditional Chinese medicine.
4. A novel method for the determination of oxymatrin and matrin in Sophora flavescens Ait. and Chinese medicine preparation by analyte focusing by micelle collapse in micellar electrokinetic chromatography. The optimal condition of the running buffer solution was 20 mmol/L sodium borate, 30 mmol /L SDS and 25% methanol at pH 9.50. The sample matrix was 30 mmol/L sodium borate and 6 mmol/L SDS. The samples were injected with pressure at 0.5 psi for 120s. The applied voltage was 20 kV and the wavelength of the detection was 205 nm.The calibration curve was linear over a range of 0.5~10μg/mL for oxymatrin and matrin, with correlation coefficients of 0.992and 0.993, respectively. The detection limits (S/N = 3:1)for oxymatrin and matrin were 0.10 and 0.20μg/ml, respectively. The relative recoveries of oxymatrin and matrin in Traditional Chinese medicine and Sophora flavescens Ait. were 94.1%~114.4%.
引文
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