快速高分离液质联用技术在农药残留检测中的应用
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摘要
随着亚二微米颗粒度色谱柱填料和新型液相色谱系统两大核心技术的突破,液质联用技术进入了全新的时代。与传统技术相比,新技术所具有的分析速度更快和分析灵敏度更高的优势将使其在未来的农药残留检测中发挥重要作用。
本论文采用快速高分离液质联用技术(RRLC-MS),针对3种农药残留体系,从样品前处理、色谱分离、质谱测定及方法的有效性等方面进行了优化和验证,建立了5个新型检测方法。
对松花江水体和饮用水中除草剂苯噻草胺及其三种光降解代谢物残留的固相萃取/快速高分离液相色谱-紫外/质谱联用(SPE/RRLC-UV/MS)和固相萃取-柱前衍生/快速高分离液相色谱-质谱联用(SPE-PCD/RRLC-MS)两种定性和定量检测方法进行了研究。在样品前处理阶段,考察了3种不同填料的固相萃取小柱和4种不同溶剂对4种分析物的吸附和洗脱回收性能;在样品分离阶段,分别采用等梯度和梯度洗脱方式,用快速分离高通量色谱柱Zorbax RRHT SB-C18 (50 mm×4.6 mm, 1.8μm, Agilent)进行分离;在定性和定量方法上,确定了每个分析物的保留时间和两对特征离子为定性参数,分别以紫外色谱和质量色谱峰面积为定量参数;同时初步研究了苯噻草胺的质谱裂解方式。两种方法对于4种分析物的线性相关系数(r2)分别为0.9992～0.9998和0.9986～0.9992,平均加标回收率为85.6%～101.4%和78.6%～101.2%,相对标准偏差(RSD)为3.0%～6.9%和3.2%～9.2%,最低检测限(LOD)为0.02μg·L~(-1)和0.02 ng·L~(-1)。实际水样品检测结果显示:松花江水体中4种化合物均为阳性检出,而饮用水中均未检到。
采用固相萃取/快速高分离液相色谱-紫外/质谱联用(SPE/RRLC-UV/MS)和固相萃取/快速高分离液相色谱-质谱/质谱联用(SPE/RRLC-MS/MS)两种分析技术对松花江水中11种三嗪类除草剂残留进行了检测。在样品前处理阶段,考察了多壁碳纳米管材料作为固相萃取吸附剂和5种不同溶剂对11种分析物的吸附和洗脱回收性能;在样品分离阶段,采用梯度洗脱方式,用快速分离高通量色谱柱Zorbax RRHT SB-C18 (50 mm×4.6 mm, 1.8μm, Agilent)进行分离;在定性和定量方法上,确定了每个分析物的保留时间和两对特征离子为定性参数,分别以紫外色谱和质量色谱峰面积为定量参数;同时初步研究了11种化合物的质谱裂解规律。两种方法对于11种分析物的线性相关系数(r2)分别为0.9992～0.9996和0.9930～0.9980,平均加标回收率分别为72.3%～97.8%和73.0%～98.0%,相对标准偏差(RSD)为3.2%～13.6%和2.6%～10.8%,最低检测限(LOD)为0.04μg·L~(-1)和0.04 ng·L~(-1)。实际水样品检测结果显示:松花江水体中11种化合物只有西玛津和莠去津为阳性检出,其他9种均未检到。
建立了果蔬品中9种有机磷类杀虫剂残留的基质固相分散萃取/快速高分离液相色谱-质谱/质谱联用(MSPD/RRLC-MS/MS)的定性和定量检测方法。考察了以多壁碳纳米管材料为基质固相分散萃取吸附剂和4种不同溶剂对9种化合物吸附和洗脱回收性能;优化了液相色谱分离和质谱测定的几个主要影响参数;初步研究了9种化合物的质谱裂解规律。该方法对于9种分析物的线性相关系数(r2)为0.9942～0.9996,平均加标回收率为71.2%～102.8%,相对标准偏差(RSD)为2.0%～11.8%,最低检测限(LOD)为0.4 ng·L~(-1),同时将该方法用于8种不同果蔬样品的实际检测。
With the breakthrough of two core techniques of sub-two micron particles chromatographic column and new liquid chromatographic system, liquid chromatography coupled to mass spectrometry (LC-MS) technology is stepping into a brand-new era. Compared with the traditional technology, praticular advantages of faster analytical speed and higher analytical sensitivity for new technology will make itself play an important role in prospective pesticide residue monitoring.
In this doctoral paper, five new analytical methods of three pesticide residue systems were developed by rapid resolution liquid chromatography coupled to mass spectrometry technology (RRLC-MS). Optimization and validation were made for four aspects of sample pre-concentration method, separation of chromatography, analysis of mass spectrum and validation of the proposed method.
Two analytical methods, SPE/RRLC-UV/MS and SPE-PCD/RRLC-MS, were investigated for the determination of herbicide mefenacet and three photolysis degradation products residues in Songhuajiang River water body and drinking water. In the SPE pre-concentration step, the adsorbent performance of three types of cartridges and the elution capability of four kinds of eluents were investigated for four analytes; in the LC separation step, rapid resolution high throughout LC column, Zorbax RRHT SB-C18 (50 mm×4.6 mm, 1.8μm, Agilent), was used and two elution modes, constant gradent and gradent, were adopted; for the qualitative and the quantitative method, the retention time and two parts of characteristic ions of every analyte were choosed to be qualitative parameters; two quantitative parameters, the peak area of UV chromatogram and mass chromatogram, were confirmed respectively and the mass spectrum fragmentation mode of mefenacet was studied. The research results show that the linear correlation coefficients (r2) of two proposed methods for four analytes are 0.9992～0.9998 and 0.9986～0.9992 respectively, the mean recoveries are 85.6%～101.4% and 78.6%～101.2% with relative standard deviations (RSD) 3.0%～6.9% and 3.2%～9.2%, the limits of detection (LOD) are 0.02μg·L~(-1) and 0.02 ng·L~(-1). The testing results for real water samples showed that four analytes were all detected in Songhuajiang River water body and were not detected in drinking water.
Two analytical methods, SPE/RRLC-UV/MS and SPE/RRLC-MS/MS, were used for the determination of eleven triazine herbicides residues in Songhuajiang River water body. In the SPE pre-concentration step, the adsorbent performance of multi-walled carbon nanotube material as SPE adsorbent and the elution capability of five kinds of eluents were investigated for eleven analytes; in the LC separation step, rapid resolution high throughout LC column, Zorbax RRHT SB-C18 (50 mm×4.6 mm, 1.8μm, Agilent), was used and the gradent elution mode was adopted; for the qualitative and the quantitative method, the retention time and two parts of characteristic ions of every analyte were choosed to be qualitative parameters; two quantitative parameters, the peak area of UV chromatogram or mass chromatogram, were confirmed respectively and the mass spectrum fragmentation law of eleven analytes was studied. The research results show that the linear correlation coefficients (r2) of two proposed methods for eleven analytes are 0.9992～0.9996 and 0.9930～0.9980 respectively, the mean recoveries are 72.3%～97.8% and 73.0%～98.0% with relative standard deviations (RSD) 3.2%～13.6% and 2.6%～10.8%, the limits of detection (LOD) are 0.04μg·L~(-1) and 0.04 ng·L~(-1). The testing results for real water samples showed that only simazine and atrazine of eleven analytes were detected in Songhuajiang River water body and other nine analytes were not detected.
MSPD/RRLC-MS/MS method was developed for the determination of nine organophosphrous pesticides residues in fruits and vegetables. The adsorbent performance of multi-walled carbon nanotube material as MSPD adsorbent and the elution capability of four kinds of eluents were investigated for nine analytes; several important parameters affecting LC separation and mass spectrum analysis were optimized; the mass spectrum fragmentation law of nine analytes was studied. The research results show that the linear correlation coefficient (r2) of the proposed method for nine analytes are 0.9942～0.9996, the mean recoveries are 71.2%～102.8% with relative standard deviation (RSD) 2.0%～11.8% , the limit of detection (LOD) is 0.4 ng·L~(-1). The proposed method was used for the simultaneous determination of these nine analytes residues in eight different fruit and vegetable samples.
本论文采用快速高分离液质联用技术(RRLC-MS),针对3种农药残留体系,从样品前处理、色谱分离、质谱测定及方法的有效性等方面进行了优化和验证,建立了5个新型检测方法。
对松花江水体和饮用水中除草剂苯噻草胺及其三种光降解代谢物残留的固相萃取/快速高分离液相色谱-紫外/质谱联用(SPE/RRLC-UV/MS)和固相萃取-柱前衍生/快速高分离液相色谱-质谱联用(SPE-PCD/RRLC-MS)两种定性和定量检测方法进行了研究。在样品前处理阶段,考察了3种不同填料的固相萃取小柱和4种不同溶剂对4种分析物的吸附和洗脱回收性能;在样品分离阶段,分别采用等梯度和梯度洗脱方式,用快速分离高通量色谱柱Zorbax RRHT SB-C18 (50 mm×4.6 mm, 1.8μm, Agilent)进行分离;在定性和定量方法上,确定了每个分析物的保留时间和两对特征离子为定性参数,分别以紫外色谱和质量色谱峰面积为定量参数;同时初步研究了苯噻草胺的质谱裂解方式。两种方法对于4种分析物的线性相关系数(r2)分别为0.9992～0.9998和0.9986～0.9992,平均加标回收率为85.6%～101.4%和78.6%～101.2%,相对标准偏差(RSD)为3.0%～6.9%和3.2%～9.2%,最低检测限(LOD)为0.02μg·L~(-1)和0.02 ng·L~(-1)。实际水样品检测结果显示:松花江水体中4种化合物均为阳性检出,而饮用水中均未检到。
采用固相萃取/快速高分离液相色谱-紫外/质谱联用(SPE/RRLC-UV/MS)和固相萃取/快速高分离液相色谱-质谱/质谱联用(SPE/RRLC-MS/MS)两种分析技术对松花江水中11种三嗪类除草剂残留进行了检测。在样品前处理阶段,考察了多壁碳纳米管材料作为固相萃取吸附剂和5种不同溶剂对11种分析物的吸附和洗脱回收性能;在样品分离阶段,采用梯度洗脱方式,用快速分离高通量色谱柱Zorbax RRHT SB-C18 (50 mm×4.6 mm, 1.8μm, Agilent)进行分离;在定性和定量方法上,确定了每个分析物的保留时间和两对特征离子为定性参数,分别以紫外色谱和质量色谱峰面积为定量参数;同时初步研究了11种化合物的质谱裂解规律。两种方法对于11种分析物的线性相关系数(r2)分别为0.9992～0.9996和0.9930～0.9980,平均加标回收率分别为72.3%～97.8%和73.0%～98.0%,相对标准偏差(RSD)为3.2%～13.6%和2.6%～10.8%,最低检测限(LOD)为0.04μg·L~(-1)和0.04 ng·L~(-1)。实际水样品检测结果显示:松花江水体中11种化合物只有西玛津和莠去津为阳性检出,其他9种均未检到。
建立了果蔬品中9种有机磷类杀虫剂残留的基质固相分散萃取/快速高分离液相色谱-质谱/质谱联用(MSPD/RRLC-MS/MS)的定性和定量检测方法。考察了以多壁碳纳米管材料为基质固相分散萃取吸附剂和4种不同溶剂对9种化合物吸附和洗脱回收性能;优化了液相色谱分离和质谱测定的几个主要影响参数;初步研究了9种化合物的质谱裂解规律。该方法对于9种分析物的线性相关系数(r2)为0.9942～0.9996,平均加标回收率为71.2%～102.8%,相对标准偏差(RSD)为2.0%～11.8%,最低检测限(LOD)为0.4 ng·L~(-1),同时将该方法用于8种不同果蔬样品的实际检测。
With the breakthrough of two core techniques of sub-two micron particles chromatographic column and new liquid chromatographic system, liquid chromatography coupled to mass spectrometry (LC-MS) technology is stepping into a brand-new era. Compared with the traditional technology, praticular advantages of faster analytical speed and higher analytical sensitivity for new technology will make itself play an important role in prospective pesticide residue monitoring.
In this doctoral paper, five new analytical methods of three pesticide residue systems were developed by rapid resolution liquid chromatography coupled to mass spectrometry technology (RRLC-MS). Optimization and validation were made for four aspects of sample pre-concentration method, separation of chromatography, analysis of mass spectrum and validation of the proposed method.
Two analytical methods, SPE/RRLC-UV/MS and SPE-PCD/RRLC-MS, were investigated for the determination of herbicide mefenacet and three photolysis degradation products residues in Songhuajiang River water body and drinking water. In the SPE pre-concentration step, the adsorbent performance of three types of cartridges and the elution capability of four kinds of eluents were investigated for four analytes; in the LC separation step, rapid resolution high throughout LC column, Zorbax RRHT SB-C18 (50 mm×4.6 mm, 1.8μm, Agilent), was used and two elution modes, constant gradent and gradent, were adopted; for the qualitative and the quantitative method, the retention time and two parts of characteristic ions of every analyte were choosed to be qualitative parameters; two quantitative parameters, the peak area of UV chromatogram and mass chromatogram, were confirmed respectively and the mass spectrum fragmentation mode of mefenacet was studied. The research results show that the linear correlation coefficients (r2) of two proposed methods for four analytes are 0.9992～0.9998 and 0.9986～0.9992 respectively, the mean recoveries are 85.6%～101.4% and 78.6%～101.2% with relative standard deviations (RSD) 3.0%～6.9% and 3.2%～9.2%, the limits of detection (LOD) are 0.02μg·L~(-1) and 0.02 ng·L~(-1). The testing results for real water samples showed that four analytes were all detected in Songhuajiang River water body and were not detected in drinking water.
Two analytical methods, SPE/RRLC-UV/MS and SPE/RRLC-MS/MS, were used for the determination of eleven triazine herbicides residues in Songhuajiang River water body. In the SPE pre-concentration step, the adsorbent performance of multi-walled carbon nanotube material as SPE adsorbent and the elution capability of five kinds of eluents were investigated for eleven analytes; in the LC separation step, rapid resolution high throughout LC column, Zorbax RRHT SB-C18 (50 mm×4.6 mm, 1.8μm, Agilent), was used and the gradent elution mode was adopted; for the qualitative and the quantitative method, the retention time and two parts of characteristic ions of every analyte were choosed to be qualitative parameters; two quantitative parameters, the peak area of UV chromatogram or mass chromatogram, were confirmed respectively and the mass spectrum fragmentation law of eleven analytes was studied. The research results show that the linear correlation coefficients (r2) of two proposed methods for eleven analytes are 0.9992～0.9996 and 0.9930～0.9980 respectively, the mean recoveries are 72.3%～97.8% and 73.0%～98.0% with relative standard deviations (RSD) 3.2%～13.6% and 2.6%～10.8%, the limits of detection (LOD) are 0.04μg·L~(-1) and 0.04 ng·L~(-1). The testing results for real water samples showed that only simazine and atrazine of eleven analytes were detected in Songhuajiang River water body and other nine analytes were not detected.
MSPD/RRLC-MS/MS method was developed for the determination of nine organophosphrous pesticides residues in fruits and vegetables. The adsorbent performance of multi-walled carbon nanotube material as MSPD adsorbent and the elution capability of four kinds of eluents were investigated for nine analytes; several important parameters affecting LC separation and mass spectrum analysis were optimized; the mass spectrum fragmentation law of nine analytes was studied. The research results show that the linear correlation coefficient (r2) of the proposed method for nine analytes are 0.9942～0.9996, the mean recoveries are 71.2%～102.8% with relative standard deviation (RSD) 2.0%～11.8% , the limit of detection (LOD) is 0.4 ng·L~(-1). The proposed method was used for the simultaneous determination of these nine analytes residues in eight different fruit and vegetable samples.
引文
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