气相色谱-串联质谱法检测蔬菜中8种氨基甲酸酯类农药残留

目的建立气相色谱-串联质谱(gaschromatography-massspectrometry,GC-MS)同时测定蔬菜样品中8种氨基甲酸酯农药残留的检测方法。方法样品加入内标溶液后,经乙腈提取,氯化钠分层,上清液用石墨化炭黑固相分散萃取净化,残留农药经DB-5MS毛细管色谱柱分离,气相色谱-质谱联用仪检测分析。结果 8种氨基甲酸酯农药在0.01～1.0μg/mL范围内的加标线性关系良好,相关系数均大于0.99,方法检出限为0.01 mg/kg,加标回收率范围在72.58%～98.48%之间,相对标准偏差为4.38%～12.63%。结论该方法灵敏度好,选择性高,操作简单,定性定量准确可靠,适合多种蔬菜样品中氨基甲酸酯农药的多残留检测。     

液相色谱双检测器串联法测定农产品中农药残留

建立了采用高效液相色谱-紫外-荧光检测器串联法测定农产品中12种农药残留的方法。采用乙腈提取,使用氨基固相萃取小柱净化,通过液相色谱柱及变换波长等各种色谱条件优化,紫外检测器检测吡虫啉、多菌灵、除虫脲、灭幼脲、辛硫磷,荧光检测器测定经柱后衍生的氨基甲酸酯类农药残留。12种农药在0.05～4mg/kg范围内线性良好,平均回收率在73.0%～108%之间,RSD为0.2%～7.1%,检出限为0.001～0.03mg/kg。方法快速、经济,为农产品中农药残留检测增加一种新思路。     

加速溶剂萃取-气相色谱-串联质谱法测定菊花中多种农药残留

目的建立一种加速溶剂萃取结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)同时检测菊花中123种农药残留的方法。方法样品采用乙腈提取,经加速溶剂萃取,石墨化碳/氨基固相萃取小柱净化,SH-Rxi-5SilMS (30 m×0.25 mm, 0.25μm)毛细管色谱柱分离,在气相色谱串联质谱多反应监测离子(multiple reaction monitoring, MRM)扫描模式下进行测定,基质外标法定量。结果在0.005～0.5mg/L范围内,123种农药有良好的线性关系(r~2≥0.9967),方法检出限为0.5～29.1μg/kg,定量下限为1.7～97.1μg/kg,在100、200、400μg/kg 3个添加水平下,123种农药的平均回收率在70.0%～128.8%之间,相对标准偏差(RSD)在0.5%～10.1%。结论该方法提取效率高、准确、灵敏,可应用于菊花中多种农药残留的筛查与测定。     

UPLC-MS/MS检测果蔬饮料中痕量吡虫啉

建立一种快速、有效的超高效液相色谱-串联质谱法测定果蔬饮料中痕量吡虫啉农药残留的方法。样品经0.1%醋酸-乙腈提取后,采用氨基固相萃取小柱进行净化和富集。采用Waters Atalantis T3色谱柱(2.1 mm×150 mm,3μm)分离,以0.1%甲酸-乙腈为流动相的梯度洗脱模式下,吡虫啉标准在0.5 ng/mL~50.0 ng/mL浓度范围内线性良好,相关系数r~2为0.999,检出限为0.15μg/kg,定量限为0.50μg/kg,加标回收率达到93.2%~96.9%。     

QuEChERS结合气相色谱-串联三重四极杆质谱快速测定水产品中100种农药残留

目的：建立Qu ECh ERS结合气相色谱-串联三重四极杆质谱快速测定水产品中100种农药残留的方法。方法：样品经改进Qu ECh ERS方法提取，分散固相萃取净化，通过气相色谱-串联三重四极杆质谱联用技术检测。结果：100种农药在0.005～0.500 mg/L范围内具有良好的线性关系，相关系数均大于0.995，对于5.00 g样品的100种农药的检出限范围为1.00×10^–6～2.97×10^–3 mg/kg，定量限范围为2.00×10^–6～9.90×10^–3 mg/kg,3个浓度添加水平的回收率在60.2%～120.0%，相对标准偏差(RSD,n=6)在0.26%～10.96%。结论：该方法具有操作简便、快速、可靠性强的特点，适用于鲩鱼、牛蛙、基围虾等水产品中多种农药残留的检测。     

薏苡仁中多种农药残留的测定

建立薏苡仁中多种杀虫剂、杀螨剂等杀菌剂农药残留的分析方法。用快速溶剂萃取仪提取,分别采用固相萃取和凝胶渗透色谱净化,气相质谱联用测定。通过固相萃取净化处理的样品添加回收率为72.45%～111.74%,RSD为1.47%～5.06%;凝胶渗透色谱处理的样品添加回收率为74.70%～106.49%,RSD为1.58%～5.08%;相关系数为0.9902～0.9995,最低检出限为0.002～0.02mg/kg,最低定量限为0.005～0.05mg/kg。方法具有高效、准确、灵敏的特点,适用于薏苡仁中多种农药残留的检测分析。     

基于PRiME-HLB的超高效液相色谱-串联质谱法测定蔬菜中43种农药残留

目的 建立基于PRiME-HLB的超高效液相色谱-串联质谱法测定蔬菜中43种农药残留的分析方法。方法 称取10 g蔬菜样品（西红柿、黄瓜、菠菜、红辣椒、生姜、韭菜、葱、土豆等8种）,以乙腈为溶剂,加入QuEChERS盐包（4 g MgSO4（无水）、1 g NaCl、0.5 g柠檬酸氢二钠、1 g柠檬酸钠）进行萃取,采用PRIME-HLB固相小柱免活化净化,与液相色谱-串联质谱技术联用,实现蔬菜中多农药残留的分析测定。结果 PRiME-HLB固相小柱能够有效降低蔬菜样品中复杂基质对农药残留检测的影响,其中70%的农药化合物属于弱基质效应;43种农药分子在5～200 μg/kg的质量浓度范围内具有良好的线性关系,相关系数(r2)均大于0.990;在实际样品中的加标回收率为60%～120%,相对标准偏差（RSD）为0.2%～10.0%;最低定量限均小于6 μg/kg。结论 该方法操作灵敏、准确可靠, 能够用于不同种类蔬菜中多种农药残留量的准确测定。     

固相萃取-气相色谱/质谱法同时测定咖啡干果皮中24种农药残留

目的:建立一种同时分析咖啡干果皮中24种农药残留的固相萃取—气相色谱/质谱方法.方法:样品用水润湿,加入乙腈提取,过Pro ElutTPC固相萃取柱净化,乙腈—甲苯(V_乙腈∶V_甲苯=3∶1)洗脱,氮吹浓缩,并采用峰面积内标法定量.结果:在28min内24种农药得到很好的分离,农药残留量为0.016～0.400 mg/kg,方法的线性良好,相关系数为0.9979～0.9999,定量限为0.01～0.03mg/kg.当农药加标水平为0.03,0.30 mg/kg时,加标回收率分别为65.2%～108.5%和81.4%～105.7%,日内精密度相对标准偏差分别为3.7%～6.8%和2.5%～5.9%,日间精密度相对标准偏差为4.2%～7.2%和2.8%～6.4%.当采用乙腈—甲苯(V_乙腈∶V_甲苯=3∶1)作洗脱溶剂、Pro ElutTPC固相萃取小柱作净化柱时,洗脱和净化效率最高,效率值为95%.结论:该方法各性能参数均满足国家标准要求,测定结果准确、可靠,能运用于咖啡干果皮中多组分农药残留的定性和定量分...     

固相萃取－液相色谱－电喷雾串联质谱法测定鲜枣中14种农药残留

选择强疏水性硅胶基质t C18柱为固相萃取净化柱,以电喷雾(ESI)为离子源,正离子多级反应离子监测(MRM)模式,建立了固相萃取-液相色谱-串联质谱法(HPLC-MS/MS)测定鲜枣中14种农药(包括有机磷杀虫剂、杀菌剂,有机杂环类杀虫剂和新型烟碱类杀虫剂)残留的分析方法。研究比较了不同提取溶剂的提取效果和不同固相萃取小柱的净化效果,同时优化了色谱分离条件和质谱条件。14种农药在10~500μg/L(或1~50μg/L)范围内线性相关,相关系数为0.996 3~0.999 9,方法的定量限为0.10~9.50μg/kg。14种农药在鲜枣中3个水平添加质量浓度的的回收率在67.4%~116.8%,RSD为0.8%~14.8%之间。该方法操作简便,灵敏度、准确度和精密度均符合农药多残留检测技术要求,适用于鲜枣中14种农药多残留的检测。     

高效液相色谱串联质谱法测定蔬菜中苯醚甲环唑的残留量

建立高效液相色谱-串联质谱检测蔬菜中苯醚甲环唑残留的分析方法。样品采用乙腈提取,经石墨碳黑-氨基串联固相萃取(GCB/NH2 SPE)柱净化,液相色谱分离多反应监测模式下测定,外标法定量。结果显示：苯醚甲环唑质量浓度在1～500ng/mL范围内线性关系良好。苯醚甲环唑在不同基质中平均回收率为79.3%～108.0%,相对标准偏差为2.7%～8.5%,检出限为0.001mg/kg。该方法灵敏度高,准确度、精密度好,满足样品测定的定性、定量要求。     

基于保留指数原理结合气相色谱-三重四极杆质谱法快速筛查蔬菜中农药残留的方法研究

目的建立气相色谱-三重四极杆质谱联用法快速筛查蔬菜中农药残留的方法。方法利用正构烷烃C9-C33标准溶液,结合气相色谱-三重四极杆质谱联用仪及其Smart Database Pesticides数据库建立仪器数据采集方法。选用9种农药为目标物,试样经QuEChERS方法进行萃取净化后,建立质谱多反应监测(multiple reaction monitoring,MRM)方法,进行定性、定量分析。结果采用空白样品添加标准溶液制得质量浓度为0.01、0.05、0.10mg/kg的样品,基于保留指数所建立的方法准确定性出待测9种农药,并测得方法的平均回收率为72.0%~118.8%。结论该方法简便、快速、成本低,具有较好的适用性,对监测农产品中农药的使用种类,更加全面合理地制定农产品中农残限量范围具有参考价值。     

QuEChERS-高效液相色谱-串联质谱法测定毛豆中常用21种农药残留

目的建立液相色谱-串联质谱法同时检测毛豆中21种常用农药残留的分析方法。方法样品以乙腈-甲酸(99:1,V:V)作为提取剂,经Qu ECh ERS方法前处理,采用Phenomenex的Kinetex C_(18)色谱柱(50 mm×2.1mm,2.6μm,100?)分离,以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,以电喷雾电离(ESI)、正离子模式和负离子模式2种多反应监测(MRM)模式检测,外标法定量。结果 21种农药在5~200 ng/m L范围内,线性相关系数均大于0.99,线性良好。分析目标物添加水平为0.01~0.10 mg/kg时,回收率范围为73%~113%,RSD范围为1.3%~10.9%,符合残留分析的要求。21种农药的定量下限为0.01 mg/kg。结论该方法的提取简便,基质分散效果好,灵敏度满足国内外限量标准的要求,适合毛豆中常用农药残留的同时测定。     

自动QuEChERS结合液相色谱-串联质谱法测定香叶中的212种农药残留

目的 建立自动QuEChERS结合液相色谱-三重四极杆串联质谱法测定香叶中212种农药残留.方法 香叶样品用乙腈提取,使用300 mg十八烷基硅烷键合硅胶(C18)+75 mg Nano-Carb、4.0 g无水硫酸镁和1.0 g氯化钠进行净化,经自动样品制备系统进行制备后,应用液相色谱-三重四极杆串联质谱法进行检测,...     

葡萄酒中17种残留农药的固相萃取-气相色谱/负化学离子源质谱测定方法研究

建立了葡萄酒中17种残留杀虫剂和杀菌剂的气相色谱～负化学离子源质谱（GC—NCI／MS）测定方法。采用C18。固相萃取小柱对葡萄酒中的残留农药进行富集,进一步完成萃取和净化,农药经乙酸乙酯洗脱后供GC—NCI／MS测定,采用基质匹配标准溶液外标法定量。验证实验表明,各农药在10-200μg／L浓度范围内线性关系良好,该方法定量检测限（S／N〉10）为5-20μg/L,在20μg,L和50μg／L处的加标回收率为70．1％-119．0％,相对标准偏差为3．5％-9．4％。该方法前处理简便快速,所采用的检测技术选择性和灵敏度高,适合葡萄酒中残留农药的测定．应用前景广阔。     

Occurrence of pesticide residues and transformation products in different types of dietary supplements

The purpose of this study was to evaluate the presence of pesticide residues and transformation products in dietary supplement products. Thirty-two samples were analysed to determine 177 pesticides by gas chromatography–tandem mass spectrometry (GC-MS/MS) and 333 pesticides by liquid chromatography–high-resolution mass spectrometry (LC-HRMS). Pesticides were extracted from different kinds of dietary supplements by the use of a modified QuEChERS extraction method. Six samples contained pesticide residues at concentration up to 92.7 µg kg^?1, but only butralin exceeded the maximum residue limits set for raw material. In addition to target compounds, LC-HRMS enables the simultaneous detection of non-target pesticides. In this case, transformation products of pesticides were detected in the analysed samples using HRMS analyser (Exactive-Orbitrap). These compounds were not included in the original method, and they were monitored as post-target compounds, knowing their molecular formula and exact mass. Mass accuracy was always < 2 ppm, corresponding to a maximum mass error. The positive findings endorse the idea that a deeper and continuous investigation of pesticide residues and transformation products in dietary supplement products is necessary in order to guaranty consumer’s safety.     

超高效液相色谱-串联质谱法测定苹果中刺糖菌素A

目的建立苹果中刺糖菌素A的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。方法样品通过乙腈匀浆提取,在电喷电离方式(ESI+)、多反应监测模式(MRM)下进行测定,基质配标准曲线定量。结果分析物在0.005~0.50 mg/kg范围内成线性,相关系数r0.99,空白样品中分析物在0.01、0.02、0.10 mg/kg三个不同添加水平时,平均回收率在93.3%~101.7%之间,相对标准偏差为5.2%~7.4%,定量限为0.005 mg/kg。结论本方法灵敏度高、准确度好,能满足定量分析的要求。     

慈溪市葡萄农药残留膳食摄入风险评估

目的开展葡萄农药残留膳食摄入风险评估工作,为葡萄食用、农药残留监管和农药最大残留限量提供科学依据。方法在2008~2013年对慈溪市生产的169批次葡萄样品进行了23种农药残留定量检测分析,分别用%ADI和%ARf D进行农药残留慢性膳食摄入风险评估和急性膳食摄入风险评估,用ADI值、大份餐和体重等参数计算最大残留限量估计值(eMRL)。结果近6年葡萄农药检出率为24.85%,超标率为0.59%。检出的7种农药慢性膳食摄入风险(%ADI)为0.010%~1.34%,平均值为0.23%;急性膳食摄入风险(%ARf D)为0.98~28.30%,平均值为8.90%。葡萄农药残留慢性膳食摄入风险和急性膳食摄入风险均很低。结论检出的7种农药最大残留限量(MRLs)均过严,建议将敌敌畏、乙酰甲胺磷、百菌清、氯氟氰菊酯、氯氰菊酯、氰戊菊酯、腐霉利等7种农药的最大残留限量分别定为0.5、3.5、2.5、2.5、2.5、2.5、11 mg/kg。     

Fast and simple extraction of pesticide residues in selected fruits and vegetables using tetrafluoroethane and toluene followed by ultrahigh-performance liquid chromatography/tandem mass spectrometry

An extraction and analytical method for the determination of pesticide residues in fruits and vegetables has been developed. The method includes extraction with a pressurised liquid solvent containing a mixture of 1,1,1,2-tetrafluoroethane and toluene, and identification/quantification of pesticides using ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry (UPLC/MS/MS). Validation studies were carried out to evaluate the performance of the method for the determination of 71 different pesticides and metabolites in tomato, cucumber, pepper, spinach, zucchini, grape, cherry, peach and apricot. Matrix-matched calibration curves were applied and correlation coefficients (r(2)) came out to be greater than 0.99. Limit of quantification (LOQ) values of the active substances were found to be lower than the maximum residue limits (MRL) according to regulations in Turkey. The recovery values were found to be between 70% and 120% with relative standard deviations less than 20%. Based on these results, the proposed method is fast, cheaper, rugged and gives quantitative results with no additional clean-up steps.     

Novel approach to fast determination of multiple pesticide residues using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).

A rapid, high-throughput method employing ultra-performance liquid chromatography with tandem quadrupole mass spectrometry (UPLC-MS/MS) was developed and optimized for simultaneous quantification and confirmation of 64 pesticide residues and their toxic metabolites in fruit extracts prepared by a buffered QuEChERS procedure. The total time required for UPLC-MS/MS analysis was 8 min plus 2 min for re-equilibration to the initial UPLC conditions. Performance characteristics were determined for apple extracts spiked at 10 microg kg(-1). The repeatability of measurements expressed as relative standard deviations was in the range 1.5-13% at this level for most analytes. Thanks to very low limits of quantification (<10 microg kg(-1)for the majority of pesticides), an optimized method allows for the reliable control of not only common maximum residue limits (MRLs) set by European Union regulation for various pesticides/fruit combinations, but also of a uniform MRL of 10 microg kg(-1)endorsed for baby food.     

Novel approach to fast determination of multiple pesticide residues using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

A rapid, high-throughput method employing ultra-performance liquid chromatography with tandem quadrupole mass spectrometry (UPLC-MS/MS) was developed and optimized for simultaneous quantification and confirmation of 64 pesticide residues and their toxic metabolites in fruit extracts prepared by a buffered QuEChERS procedure. The total time required for UPLC-MS/MS analysis was 8 min plus 2 min for re-equilibration to the initial UPLC conditions. Performance characteristics were determined for apple extracts spiked at 10 microg kg(-1). The repeatability of measurements expressed as relative standard deviations was in the range 1.5-13% at this level for most analytes. Thanks to very low limits of quantification (<10 microg kg(-1)for the majority of pesticides), an optimized method allows for the reliable control of not only common maximum residue limits (MRLs) set by European Union regulation for various pesticides/fruit combinations, but also of a uniform MRL of 10 microg kg(-1)endorsed for baby food.