GPC-GC-MS/MS法测定食用植物油中抗氧化剂BHA、BHT和TBHQ

该试验建立了食用植物油中抗氧化剂BHA、BHT和TBHQ的凝胶渗透色谱(GPC)净化-气相色谱三重四极杆串联质谱(GC-MS/MS)分析方法.样品经凝胶渗透色谱净化,用气相色谱三重四极杆串联质谱分析测定.结果 显示:在5～100 mg/L的质量浓度范围内各组分具有良好的线性关系,相关系数R在0.9991以上;BHA、B...     

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,...     

多壁碳纳米管小柱-液质联用法测定鸡肉中兽药残留方法的研究

本实验建立了鸡肉中喹诺酮类、磺胺类、氯霉素类、四环素类兽药残留的液相色谱-串联质谱快速测定方法.研究了鸡肉中4类兽药残留的提取、净化前处理条件,试样用2.5％甲酸乙腈溶液提取,滤过型多壁碳纳米管小柱净化,Accucore VDX色谱柱梯度分离,三重四极杆质谱测定,基质标准曲线法定量.同时以电喷雾离子源正模式和负模式扫描...     

气相色谱-三重四极杆质谱法测定稻米中27种持久性有机污染物

目的 建立气相色谱-三重四极杆质谱法测定稻米样品中多氯联苯、有机氯农药和多溴联苯醚等27种持久性有机污染物的分析方法.方法 糙米粉样品经水化后,采用乙酸乙酯进行2次直接提取,采用5 g酸性硅胶(44％,m∶m)固相净化柱进行净化后采用气相色谱-三重四极杆质谱在动态多反应离子监测模式进行分析,内标法定量.结果 27种持久...     

QuEChERS/超高效液相色谱-串联质谱法测定大黄鱼中非法染料硫代黄素

建立了超高效液相色谱-串联质谱法测定大黄鱼中硫代黄素残留的分析方法.样品中的硫代黄素经乙腈-水溶液提取,QuEChERS方法净化,C18色谱柱分离,以0.1％(体积分数)甲酸水溶液-乙腈为流动相进行梯度洗脱,三重四极杆质谱电喷雾多反应监测模式检测,外标法定量.结果表明,硫代黄素为0.5～50.0 ng/mL时线性关系良...     

固相萃取-液相色谱-串联质谱法测定牛奶中辛基酚和正辛基酚

建立了牛奶中辛基酚和正辛基酚的液相色谱-串联三重四极杆质谱测定方法.样品经氨水乙腈(1:9,体积比)溶解,超声提取,PRiME HLB固相萃取柱净化后,经安捷伦Poroshell 120 PFP色谱柱(100 mm×4.6 mm,2.7 μm)分离,采用多反应监测负离子模式监测,内标法定量.在该优化条件下,牛奶中辛基酚...     

超高效液相色谱-三重四极杆质谱联用法同时测定粮谷类食品中的5种真菌毒素

目的建立一种一步式净化柱净化、超高效液相色谱-三重四极杆质谱联用法同时测定粮谷类食品中黄曲霉毒素B_1、B_2、G_1、G_2、玉米赤霉烯酮5种真菌毒素的分析方法。方法以84%(V:V)乙腈作为提取溶剂,样品经均质后经一步式多功能净化柱净化后进超高效液相色谱-三重四极杆质谱联用仪,利用C_(18)色谱柱分离,采用电喷雾离子源(electrospray ionization,ESI)和多反应监测模式(multiple reaction monitoring mode,MRM),在正、负离子模式下同时进行定性定量测定。结果 5种真菌毒素目标分析物在各自的质量测定浓度范围内,线性相关系数良好(相关系数r~2 0.999),方法定量限为0.10～4.00μg/kg,加标回收率为73.5%～112.5%,相对标准偏差小于15%。结论该方法前处理操作简便,灵敏度高,定性定量准确,可满足对粮谷类产品中多种真菌毒素同时检测的要求。     

高效液相色谱-串联质谱法快速检测植物药酒中的40种生物碱

目的 建立高效液相色谱-串联三重四极杆质谱(high performance liquid chromatography-tandem triple quadrupole mass spectrometry,HPLC-MS/MS)法快速检测植物药酒中40种生物碱的分析方法.方法 样品采用乙腈提取,提取液经N-丙基乙二胺...     

安捷伦科技推出新款三重串联四极杆LC／MS系统，可升级满足未来需求

2011年6月6日．安捷伦科技公司（纽约证交所A）推出Agilent6420三重串联四极杆液相色谱／质谱（LC／MS）系统．这是一款全新打造的高负荷三重串联四极杆系统．可随客户需求变化轻松升级至性能更高的6430和6460系统。     

基于UPLC-MS-MS技术快速测定花生中4种黄曲霉毒素

建立了花生中4种黄曲霉毒素的超高液相色谱-三重四极杆串联质谱(UPLC-MS-MS)检测的方法。样品经80%乙腈-水溶液振荡超声提取后,采用多功能净化柱净化。待测物经Kinetex SB-C18色谱柱分离,甲醇-0.1%甲酸溶液为流动相,梯度洗脱,三重四级杆串联质谱多反应离子监测(MRM)方式检测,外标法定量。结果表明:4种黄曲霉毒素在各自的线性响应范围内线性关系良好,相关系数均大于0.999,方法的检出限为0.014~0.025μg/kg,空白样品中加标回收率为72.25%~89.46%,RSD在4.01%~9.56%之间。该方法前处理简单快速、净化效果好、检出限低,适合花生中多种黄曲霉毒素的同时快速测定。     

液相色谱串联质谱法测定肉中丙硫咪唑及其代谢物

建立同时测定肉中丙硫咪唑及其代谢物丙硫咪唑砜、丙硫咪唑亚砜、2-氨基丙硫咪唑砜的液相色谱串联质谱法。样品用乙腈提取,液液分配净化后,XDB-C18色谱柱分离,流动相乙腈:0.1%甲酸溶液(1:1,V/V),外标法定量。丙硫咪唑及其3种代谢物的检出限均为0.010mg/kg,在0.010～1.0mg/L范围内其质量浓度与峰面积呈良好的线性关系,相关系数大于0.99。添加量为0.010～0.050mg/kg时的回收率为82.3%～97.6%,相对标准偏差为4.9%～12.9%。该方法简便、快速、准确,可用于猪肉、牛肉、羊肉、鸡肉、香肠中丙硫咪唑及其代谢物的定性、定量检测。     

Determination of pesticides and their metabolites in processed cereal samples

Fifteen pesticides including some of their metabolites (disulfoton sulfoxide, ethoprophos, cadusafos, dimethoate, terbufos, disulfoton, chlorpyrifos-methyl, malaoxon, fenitrothion, pirimiphos-methyl, malathion, chlorpyrifos, terbufos sulfone, disulfoton sulfone and fensulfothion) were analysed in milled toasted wheat and maize as well as in wheat flour and baby cereals. The QuEChERS (quick, easy, cheap, effective, rugged and safe) methodology was used and its dispersive solid-phase extraction procedure was optimised by means of an experimental design with the aim of reducing the amount of co-extracted lipids and obtaining a clean extract. Gas chromatography with nitrogen phosphorus detection were used as the separation and detection techniques, respectively. The method was validated in terms of selectivity, recoveries, calibration, precision and accuracy as well as matrix effects. Limits of detection were between 0.07 and 34.8 μg kg(-1) with recoveries in the range of 71-110% (relative standard deviations were below 9%). A total of 40 samples of different origin were analysed. Residues of pirimiphos-methyl were found in six of the samples at concentrations in the range 0.08-0.47 mg kg(-1), which were below the MRLs established for this pesticide in cereal grains. Tandem mass spectrometry confirmation was also carried out in order to identify unequivocally the presence of this pesticide.     

气相色谱-负化学源-质谱法测定茶叶中的氟虫腈及其代谢物

建立气相色谱-负化学源-质谱法测定茶叶中氟虫腈及其代谢物：氟甲腈、氟虫腈砜和氟虫腈亚砜。采用乙腈提取茶叶中的氟虫腈及其代谢物，并通过正己烷液液分配后，经PSA-SPE柱净化。采用气相色谱-负化学源-质谱法进行氟虫腈及其代谢物的检测，外标法定量。结果表明，茶叶中的氟虫腈及其代谢物在16 min内被分离。方法中4种目标物的线性范围为0.002～0.200?μg/mL，相关系数R²>0.999，检出限(R_SN=10)为0.002 mg/kg，相对标准偏差低于5%。在添加量为0.002、0.010 mg/kg和0.020 mg/kg时，加标回收率在96.33%～102.50%之间。本方法线性范围广、准确性高、重复性好，可以快速准确地对市售茶叶中氟虫腈及其代谢物进行痕量检测分析。     

Determination of pesticides and their metabolites in processed cereal samples

Fifteen pesticides including some of their metabolites (disulfoton sulfoxide, ethoprophos, cadusafos, dimethoate, terbufos, disulfoton, chlorpyrifos-methyl, malaoxon, fenitrothion, pirimiphos-methyl, malathion, chlorpyrifos, terbufos sulfone, disulfoton sulfone and fensulfothion) were analysed in milled toasted wheat and maize as well as in wheat flour and baby cereals. The QuEChERS (quick, easy, cheap, effective, rugged and safe) methodology was used and its dispersive solid-phase extraction procedure was optimised by means of an experimental design with the aim of reducing the amount of co-extracted lipids and obtaining a clean extract. Gas chromatography with nitrogen phosphorus detection were used as the separation and detection techniques, respectively. The method was validated in terms of selectivity, recoveries, calibration, precision and accuracy as well as matrix effects. Limits of detection were between 0.07 and 34.8?µg?kg^?1 with recoveries in the range of 71–110% (relative standard deviations were below 9%). A total of 40 samples of different origin were analysed. Residues of pirimiphos-methyl were found in six of the samples at concentrations in the range 0.08–0.47?mg?kg^?1, which were below the MRLs established for this pesticide in cereal grains. Tandem mass spectrometry confirmation was also carried out in order to identify unequivocally the presence of this pesticide.     

快速滤过型净化结合液相色谱-质谱联用法测定海产品中19种磺胺类药物残留

建立了快速滤过型净化(m-PFC,multi-plug filtration cleanup)结合液相色谱-质谱联用技术同时检测海产品中19种磺胺类药物的分析方法。样品加水浸润后经过甲酸乙腈提取,QuEChERS盐包分层,取上层提取液经m-PFC柱净化,液相色谱-质谱联用测定,采用多反应监测模式(MRM)进行分析,基质外标法定量。结果表明,19种磺胺类药物在1～100μg/L的范围内线性关系良好,决定系数大于0.997,检出限为0.005～0.15μg/kg,定量限为0.01～0.41μg/kg。在10、20、100μg/kg三水平的平均添加回收率为70.0%～114.1%,相对标准偏差为0.5%～9.4%。该方法操作简便、快速,灵敏度高,重现性好,适用于海产品中多种磺胺类药物残留的检测。     

多壁碳纳米管磁性固相萃取气相色谱质谱法测定茶叶中的8种农药残留

建立了磁性固相萃取-气相色谱质谱法测定茶叶中8种农药的检测方法,利用乙腈对样品进行提取,使用磁性吸附剂MWCNTs-Fe3O4富集和净化茶叶初提液中的农药,气相色谱-质谱定量检测.对影响磁性固相萃取的条件进行了优化,主要包括萃取剂、吸附剂用量、吸附时间、洗脱剂、洗脱时间等.结果 表明,8种农药在各自质量浓度范围内线性关...     

QuEChERS-高效液相色谱-串联质谱法测定牛奶中氨基甲酸酯类农药残留量

目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定牛奶中5种氨基甲酸酯类农药的方法。方法样品经乙腈提取、氮吹浓缩、QuEChERS净化,高效液相色谱-串联质谱法测定,采用外标法定量。结果5种氨基甲酸酯类农药在2.00-200μg/kg范围内线性关系良好(r>0.999);方法检出限为0.50~3.00μg/kg,定量限为1.50~10.00μg/kg;加标水平为0.010~0.050 mg/kg时,回收率为83.6%-108%,相对标准偏差为1.6%~15.6%。结论该方法简便快捷、灵敏度高,适用于牛奶中氨基甲酸酯类农药的检测。     

分散固相萃取-气相色谱-串联质谱法测定茉莉花茶中86种农药残留

以QuEChERS（Quick,Easy,Cheap,Effective,Rugged,Safe）法为前处理技术,优化净化吸附剂组合和用量,改进净化方式,并以气相色谱-串联质谱（gas chromatography-tandem mass spectrometry,GC-MS/MS）法为检测手段,建立茉莉花茶中86 种农药残留筛查检测方法。样品用乙腈提取,提取液经饱和的氯化钠溶液萃取,取有机相,转移至装有混合吸附剂和有机滤膜的针筒中完成净化与过滤,GC-MS/MS测定,外标法定量。86 种农药线性范围在5～400 μg/kg之间线性关系良好,相关系数（r2）在0.98以上,方法定量限为0.1～8.0 μg/kg。当添加水平为80 μg/kg时,91.8%的农药平均加标回收率在70.1%～116.0%之间,相对标准偏差为1.9%～11.4%。     

多壁碳纳米管QuEChERS-气相色谱法测定茶叶中23 种有机磷农药残留量

建立测定茶叶中23 种有机磷农药残留量的气相色谱检测方法。茶叶样品经丙酮提取后,采用QuEChERS方法前处理,以N-丙基乙二胺（N-propyl ethylenediamine,PSA）、多壁碳纳米管（multi walled carbon nanotubes,MWCNTs）吸附提取液中的干扰组分,净化液经气相色谱测定,基质外标法定量。采用本实验建立的方法,在0.02～1.00?μg/mL范围内,23?种有机磷的线性关系良好,相关系数r大于0.986?5,方法检出限为0.01～0.02?mg/kg,定量限为0.03～0.06?mg/kg。在0.05、0.50、1.00?mg/kg三个添加量的平均加标回收率为81.8%～107.2%,相对标准偏差为1.2%～7.2%。与传统的QuEChERS相比,该方法具有操作简单、快速、试剂用量少、回收率高、准确性强等特点,适合于茶叶中23?种有机磷农药残留量的测定。     

Pepper leaf matrix as a promising analyte protectant prior to the analysis of thermolabile terbufos and its metabolites in pepper using GC–FPD

During gas chromatography (GC), the matrix can deactivate the active site during the transport of the compound from the injector to the detector. This deactivation capacity varies among matrices, as it is dependant on the concentrations of the different constituent compounds of each matrix. During the analysis of terbufos and its metabolites, two of its metabolites were highly thermolabile, and were readily decomposed inside the GC system. As the matrix can mask the active site, we carried out a matrix-matched calibration in an effort to protect the analyte against decomposition. As a component of our analysis, the pepper matrix was the first to be matched; however, it failed to completely protect the metabolites. Subsequently, a variety of different compounds, including 3-ethoxy-1,2-propanediol, gulonolactone, and sorbitol at 10, 1, and 1 mg/mL were tested; however, none of these generated the desired effect. We surmised that some of the compounds may have decomposed inside the injection port, so we introduced a carbofrit inlet liner, which is highly inert. But, this step did not improve the protective qualities of the matrices. Finally, pepper leaf matrix was added to the pepper matrix, and we observed a profound protective effect for almost all of the analytes tested. A selective detector (flame photometric detector with phosphorus filter) was used to facilitate a high matrix concentration without interaction with the analyte. After resolving the problem of these two metabolites, terbufos and its five toxic metabolites were analyzed in pepper and pepper leaf samples. The recovery rates for terbufos and its metabolites were 73–114.5% with a relative standard deviation of <12%. This method was successfully applied to field samples, and terbufos sulfone, terbufos sulfoxide, and terbufoxon sulfoxide were found as residues in the suspected pepper and pepper leaf samples.