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基质固相萃取-气相色谱电子捕获检测器同时测定大米中12种有机氯农药残留量 总被引:4,自引:0,他引:4
建立了大米中12种有机氯农药气相色谱-电子捕获检测器检测方法.采用基质固相分散(Matrix Solid Phase Disperse, MSPD)技术进行样品前处理, 用气相色谱-电子捕获检测器进行快速定性定量分析.基质固相分散集提取、过滤、净化于一步完成, 避免了样品均化、转溶、乳化、浓缩造成的待测农药组分的损失, 大大提高了方法的准确度和精密度.12种有机氯农药的添加回收率在83%~103%之间,相对标准偏差为2.2%~19%. 相似文献
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适量水浸润的铁皮石斛样品经乙腈高速涡旋和超声提取。离心后,上清液采用分散固相萃取净化,吸附剂为C18和N-丙基乙二胺。采用分散固相萃取-气相色谱-串联质谱法测定净化液中41种农药的残留量。在气相色谱分离中采用Agilent VF-5MS色谱柱,在串联质谱分析中采用多反应监测模式。以外环氧七氯为内标,41种农药的检出限(3S/N)为0.001~0.024 mg·kg~(-1)。以空白样品为基体进行加标回收试验,所得回收率为75.1%~115%,测定值的相对标准偏差(n=6)为0.40%~11%。 相似文献
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分散固相萃取-气相色谱-串联质谱法测定蔬菜中107种农药的残留量 总被引:11,自引:0,他引:11
采用分散固相萃取-气相色谱-串联质谱(QuEChERS-GC-MS/MS)建立了蔬菜中107种农药残留量的分析方法。样品由含1%冰醋酸的正己烷饱和乙腈提取、分散固相萃取法净化,采用气相色谱-串联质谱方法在分时段选择反应监测模式下进行测定,外标法定量。所有农药在0.05~1 mg/L范围内线性关系均良好;所有农药的方法定量限(LOQ)均低于10 μg/kg;在10 μg/kg的添加水平下,大蒜、青刀豆、萝卜和菠菜4种基质中绝大多数农药的平均回收率处于60%~130%之间,相对标准偏差(RSD)不大于15.3%。该方法不仅能用于多种蔬菜基质中107种农药残留的检测,而且还能较好地解决本底成分相当复杂的大蒜基质极易出现的干扰问题。 相似文献
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建立了分散固相萃取-气相色谱测定对虾中12种有机磷农药残留的分析方法。样品经V(冰乙酸):V(乙腈)=1:99溶液提取,采用乙二胺-N-丙基硅烷(PSA)、C18与石墨炭黑(GCB)为吸附剂进行分散固相萃取净化。以DB-17毛细管色谱柱分离,GC-FPD(P)检测。方法在0.01~0.50μg/mL范围内线性关系良好,相关系数(r2)均不低于0.9971,12种有机磷农药的方法检出限均为0.01 mg/kg。在0.01~0.10 mg/kg的添加水平下,平均加标回收率为80.7%~101.2%,相对标准偏差为3.7%~7.6%。 相似文献
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气相色谱-负化学离子源质谱测定大豆和玉米中12种三唑类杀菌剂的残留量 总被引:2,自引:0,他引:2
建立了一种可用于大豆和玉米中12种三唑类杀菌剂残留量测定的分散固相萃取-气相色谱-负化学离子源质谱方法。样品经含1%冰醋酸的乙腈提取,分散固相萃取法净化,采用气相色谱-负化学离子源质谱分时段选择离子监测技术进行测定与确证,外标法定量。12种农药在50~1000 μg/L范围内线性关系均良好;所有农药的方法定量限(LOQ)均低于8 μg/kg;在10,20和40 μg/kg 3个添加水平下所有农药的回收率为70%~130%,相对标准偏差(RSD)≤13.9%。该方法在检测大豆和玉米基质时无干扰现象出现。 相似文献
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分散固相萃取气相色谱-负化学离子源质谱法测定大豆和玉米中20种农药的残留量 总被引:8,自引:0,他引:8
建立了一种大豆和玉米中20种农药残留量的分散固相萃取气相色谱-负化学离子源质谱分析方法。样品经乙腈提取并浓缩后加入N-丙基乙二胺(PSA)、石墨化碳黑和C18 3种填料进行分散固相萃取净化,气相色谱-负化学离子源质谱分时段选择离子监测技术测定与确证,外标法定量。所有农药在20~400 μg/L范围内线性均良好;方法的定量限(LOQ)均不高于2 μg/kg;在5,10和20 μg/kg 3个添加水平下所有农药的平均回收率均处于70%~130%之间,相对标准偏差(RSD)低于17%;运用该方法检测大豆和玉米样品时没有干扰现象。 相似文献
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气相色谱-电子轰击离子源质谱法分析卷烟和烟叶中29种农药的残留 总被引:7,自引:1,他引:6
开展了卷烟和烟叶中有机氯、有机磷和拟除虫菊酯3类29种农药残留的气相色谱-电子轰击离子源质谱(GC-EI/MS)的分析方法研究。优化与选择了卷烟和烟叶样品的前处理条件,样品经正己烷-丙酮(体积比为1∶1)混合提取剂超声提取、Florisil硅土和中性氧化铝双净化剂固相萃取柱净化、二氯甲烷-正己烷(体积比为95∶5)混合洗脱剂洗脱和浓缩后,以磷酸三苯酯(TPP)为内标物,采用GC-EI/MS的选择离子监测方式(SIM)进行定性和定量分析。当样品的加标水平为20,50,100 μg/kg时,加标回收率为70%~110%,相对标准偏差在2%~8%之间;除了甲氰菊酯、氯菊酯和溴氰菊酯的方法检出限(LOD)分别为1.85,1.74与2.54 μg/kg外,其余的26种农药的LOD均小于0.8 μg/kg;线性范围为5.0~500.0 μg/kg,相关系数都大于等于0.9994。此分析方法已成功地应用于卷烟和烟叶样品中3类29种痕量农药残留的分析 相似文献
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气相色谱-质谱法分析蜂蜜中的多种农药残留 总被引:2,自引:0,他引:2
开展了蜂蜜中23种农药残留的气相色谱-电子轰击离子源质谱(GC-EI/MS)分析方法的研究,并对其中3种农药的EI/MS碎片离子的断裂机理与结构进行了初步解析。探讨了蜂蜜试样前处理条件的优化与选择。将蜂蜜试样用乙酸乙酯提取剂超声提取、Florisil硅藻土色谱柱净化和正己烷-乙酸乙酯(体积比为7∶3)混合洗脱剂洗脱后,以PCB103为内标物,采用选择离子监测(SIM)方式下的GC-EI/MS分析。当试样的加标浓度为50,100和200 μg/kg时,加标回收率为82%~120%,相对标准偏差小于11.0%。23种农药的检测限都小于10.0 μg/kg,线性范围为10~500 μg/kg,相关系数都大于0.995。此分析方法已成功地应用于蜂蜜中23种痕量农药残留的分析。 相似文献
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Xiaoyan Xia Bernard S. Crimmins Philip K. Hopke James J. Pagano Michael S. Milligan Thomas M. Holsen 《Analytical and bioanalytical chemistry》2009,395(2):457-463
Toxaphene is considered to be a problematic organochlorine pollutant because of its bioaccumulation potential and persistence
in aquatic environments. In this study, whole lake trout and walleye composites were used to evaluate two analytical techniques
for total toxaphene and selected congener analysis. The efficacy of using gas chromatography electron ionization tandem mass
spectrometry (GC-EI/MS/MS) and electron capture negative ionization mass spectrometry (GC-ECNI-MS) were compared. Although
the sensitivity using GC-ECNI-MS was approximately five times greater than GC-EI/MS/MS, the latter provided more consistent
inter-Parlar relative response factors (RRF). When using technical calibration mixtures, these results suggest a more accurate
total toxaphene measurement was obtained using the GC-EI/MS/MS method. Total toxaphene concentrations in lake trout composites
from both methods were highly correlated (R
2 = 0.985) with the MS/MS concentrations approximately half of those determined by ECNI, suggesting systematic high bias in
toxaphene concentrations when measured using GC-ECNI. 相似文献
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Hasnae Garoiaz Mohammed Berrabah Abderahmane Elidrissi Belkheir Hammouti 《International journal of environmental analytical chemistry》2013,93(12):1378-1388
A fast, simple and inexpensive sample preparation method based on the matrix solid-phase extraction (SPE) technique is proposed for the isolation of cypermethrin and its metabolite residues from soils. Both the extraction and clean-up procedures were carried out in two steps and target compounds were determined by gas chromatography coupled with electron-impact mass spectrometry (GC-EI/MS). The characteristic ions and fragmentation mechanism of cypermethrin were evaluated by electron impact ionization mass spectrometry (EI/MS). After the optimization of different parameters, such as the extraction solvent, the pesticide was extracted from the matrix with methanol/acetone in a Soxhlet extractor, cleaned up on a Florisil column by elution with a mixture of 30% ethyl acetate in n-hexane and analyzed by gas chromatography-electron impact ionization mass spectrometry (GC-EI/MS) in the selected ion-monitoring mode (SIM) with permethrin as internal standard. Recovery was in the range 77–118% with relative standard deviations (RSD) between 2.5% and 10.2%. The limit of detection (LOD) was 6.5?µg/kg for cypermethrin. The developed method was linear in the injection range 6–30?ng, with correlation coefficients greater than 0.9957. 相似文献
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Steven G. O’Connell Theodore Haigh Glenn Wilson Kim A. Anderson 《Analytical and bioanalytical chemistry》2013,405(27):8885-8896
We developed two independent approaches for separation and quantitation of 24 oxygenated polycyclic aromatic hydrocarbons (OPAHs) using both liquid chromatography-atmospheric pressure chemical ionization/mass spectrometry (LC-APCI/MS) and gas chromatography-electron impact/mass spectrometry (GC-EI/MS). Building on previous OPAH research, we examined laboratory stability of OPAHs, improved existing method parameters, and compared quantification strategies using standard addition and an internal standard on an environmental sample. Of 24 OPAHs targeted in this research, 19 compounds are shared between methods, with 3 uniquely quantitated by GC-EI/MS and 2 by LC-APCI/MS. Using calibration standards, all GC-EI/MS OPAHs were within 15 % of the true value and had less than 15 % relative standard deviations (RSDs) for interday variability. Similarly, all LC-APCI/MS OPAHs were within 20 % of the true value and had less than 15 % RSDs for interday variability. Instrument limits of detection ranged from 0.18 to 36 ng mL?1 on the GC-EI/MS and 2.6 to 26 ng mL?1 on the LC-APCI/MS. Four standard reference materials were analyzed with each method, and we report some compounds not previously published in these materials, such as perinaphthenone and xanthone. Finally, an environmental passive sampling extract from Portland Harbor Superfund, OR was analyzed by each method using both internal standard and standard addition to compensate for potential matrix effects. Internal standard quantitation resulted in increased precision with similar accuracy to standard addition for most OPAHs using 2-fluoro-fluorenone-13C as an internal standard. Overall, this work improves upon OPAH analytical methods and provides some considerations and strategies for OPAHs as focus continues to expand on this emerging chemical class. Figure
OPAH chromatograms from GC-EI/MS and LC-APCI/MS methods for NIST SRM 1650b (diesel particulate matter) 相似文献
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气相色谱-质谱法同时测定动物内脏中的14种酞酸酯类环境激素残留 总被引:2,自引:0,他引:2
开展了动物内脏中14种酞酸酯类(PAEs)环境激素残留的气相色谱-电子轰击离子源/质谱(GC-EI/MS)的分析方法研究。优化与选择了动物内脏样品的前处理条件,动物内脏样品经正己烷/二氯甲烷(1/1,v/v)混合提取剂超声提取、Florisil硅藻土固相萃取柱净化与乙酸乙酯/正己烷(2/3,v/v)混合洗脱剂洗脱和浓缩后,以邻苯二甲酸二苯基酯(DPhP)为内标物,采用GC-EI/MS的选择离子监测方式(SIM)进行定性和定量分析。当猪肝样品的加标浓度水平为100、200、400 μg/kg时,加标回收率为:60%~110%,相对标准偏差为:0.78%~10.3%;除邻苯二甲酸二(2-甲氧基乙基)酯(DMEP)与邻苯二甲酸二(2-乙氧基乙基)酯(DEEP)的检测限(MDL)分别为3.30与2.25 μg/kg外,其余的12种PAEs的MDL ≦ 1.74 μg/kg;线性范围为50 ~ 800 μg/kg,相关系数都大于0.9994。此分析方法成功地应用于6种动物内脏中14种痕量PAEs残留的分析。 相似文献
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Gouveia CA Oliveira A Pinho S Vasconcelos C Carvalho F Moreira RF Dinis-Oliveira RJ 《Biomedical chromatography : BMC》2012,26(8):1041-1047
The development of analytical techniques that enable the use of hair as an alternative matrix for the analysis of drugs of abuse is useful for confirming the exposure in a larger time window (weeks to months, depending on the length of the hair shaft). In the present study a methodology aimed at the simultaneous quantification of cocaine and morphine in human hair was developed and validated. After decontamination, hair samples (20?mg) were incubated with a mixture of methanol/hydrochloric acid (2:1) at 65?°C overnight (~16?h) in order to extract the drugs of the matrix. Purification was performed by solid-phase extraction using mixed-mode extraction cartridges. After derivatization with N-methyl-N-(trimethylsilyl) trifluoroacetamide, blank, standards and samples were analyzed by gas chromatography/electron impact-mass spectrometry (GC-EI/MS). The method proved to be selective, as there were no interferences of endogenous compounds with the same retention time as cocaine, morphine and ethylmorphine (internal standard). The regression analysis for both analytes showed linearity in the range 0.25-10.00?ng/mg with correlation coefficients ranging from 0.9989 to 0.9991. The coefficients of variation oscillated between 0.83 and 14.60%. The limits of detection were 0.01 and 0.02?ng/mg, and the limits of quantification were 0.03 and 0.06?ng/mg for cocaine and morphine, respectively. The proposed GC-EI/MS method provided an accurate and simple assay with adequate precision and recovery for the quantification of cocaine and morphine in hair samples. The proof of applicability was performed in hair samples obtained from drug addicts enrolled in a Regional Detoxification Treatment Center. The importance of hair samples is highlighted, since positives results were obtained when urine immunoassay analyses were negative. Copyright ? 2012 John Wiley & Sons, Ltd. 相似文献
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Pihlström T Blomkvist G Friman P Pagard U Osterdahl BG 《Analytical and bioanalytical chemistry》2007,389(6):1773-1789
A multiresidue method based on extraction with ethyl acetate has been used at the Swedish National Food Administration since
1989 to monitor pesticide residues in fruit and vegetables. The method has been continuously adjusted, resulting in simple
and quick analyses of pesticide residues. To recover basic pesticides, the addition of an alkali is necessary. The addition
of sodium hydrogen carbonate has been shown to recover all pesticides effectively without any degradation. The liquid chromatography
(LC) with tandem mass spectrometry (MS/MS) technique has made it possible to analyse more polar pesticides and to replace
many single methods. The latest development in the multiresidue method, comprising the use of gas chromatography (GC) with
MS/MS, has further improved the analysis by replacing the conventional GC detectors. The need for cleanup has been reduced
or eliminated entirely. Consequently, the method has been simplified in a way that makes it possible to recover all included
analytes in many different matrices in one single extraction and to detect them either with GC-MS/MS or with LC-MS/MS. 相似文献
20.
High-throughput GC/MS and HPLC/MS/MS techniques for the multiclass, multiresidue determination of 653 pesticides and chemical pollutants in tea 总被引:1,自引:0,他引:1
Pang GF Fan CL Zhang F Li Y Chang QY Cao YZ Liu YM Li ZY Wang QJ Hu XY Liang P 《Journal of AOAC International》2011,94(4):1253-1296
An efficient and sensitive method has been established for simultaneous determination of 653 pesticides in teas by GC/MS and HPLC/MS/MS. The method involved extraction with acetonitrile followed by cleanup using Cleanert-TPT SPE and subsequent identification and quantitation of 490 pesticides by GC/MS and 448 pesticides by HPLC/MS/ MS. The LODs for pesticides determined by GC/MS were between 1.0 and 500 microg/kg, and those determined by HPLC/MS/MS were between 0.03 and 4820 microg/kg. At the low fortification levels of 0.01-100 microg/kg, the average recoveries of 94% of the pesticides determined by GC/MS were between 60 and 120%, 77% of which had an RSD below 20%. For 91% of pesticides determined by HPLC/MS/MS, the average recoveries were between 60 and 120%, 76% of which had an RSD below 20%. The paper also reports a novel SPE column, Cleanert TPT, which comprised graphitized carbon black (PestiCarb), polyamine silica, and amide polystyrene for purifying the tea samples. The results indicated good repeatiblity and reproducibility. 相似文献