共查询到20条相似文献,搜索用时 15 毫秒
1.
Esteve-Turrillas FA Pastor A de la Guardia M 《Analytical and bioanalytical chemistry》2006,384(3):801-809
A comparative study was carried out for the simultaneous determination of 11 pyrethroid insecticides in soil by gas chromatography
(GC) - ion trap (IT)- mass spectrometry (MS), by means of two different ionization modes; electron impact and negative chemical
ionization and three data acquisition procedures; full scan, selected ion monitoring and MS/MS. Pyrethroids investigated were
tetramethrin, bifenthrin, phenothrin, λ-cyhalothrin, permethrin, cyfluthrin, cypermethrin, flucythrinate, esfenvalerate, fluvalinate
and deltamethrin. Soil samples were treated with toluene/water by microwave-assisted extraction for 9 min at 700 W and a cleaning
up with florisil was performed. Clean soil samples were spiked with pyrethroids at a spiking level of 10, 25 and 50 ng/g.
The method employed provides a concentration factor of 10. The ionization gas employed in the negative chemical ionization
mode was methane. The use of MS/MS acquisition, in electron impact ionization, provided the best results, due to its high
selectivity and sensitivity, giving very low limits of detection from 0.08 to 0.54 ng/g. In negative chemical ionization full
scan and selected ion monitoring methods detection limits from 0.12 to 1.40 ng/g were found. The proposed methods were applied
to several levels from 10 to 50 ng/g of spiked soils, being electron impact MS/MS method which minimizes matrix spectrum interferences
and provided recovery average values from 84% to 120% with relative standard deviations which varied from 3.2 to 7.2%. 相似文献
2.
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
3.
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
4.
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
5.
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
6.
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
7.
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
8.
建立了微波辅助萃取结合气相色谱-飞行时间质谱(GC-TOF MS)技术在负化学电离(NCI)源和电子轰击电离(EI)源两种模式下测定烟草中24种农药残留的分析方法。烟叶样品于100℃下用二氯甲烷-正己烷(3:1, v/v)混合溶剂微波萃取10 min,萃取液经弗罗里硅土固相萃取柱净化后进行检测分析。在NCI源和EI源质谱模式下,24种农药的线性关系均良好(r2>0.99),相对标准偏差分别小于8.6%和9.1%,定量限分别为0.3~6.9 μg/kg和10.2~44.9 μg/kg,加标回收率分别为75.2%~94.8%和75.0%~95.1%。比较两种离子源模式下的色谱图和质谱图,NCI源模式较EI源模式的选择性好、灵敏度高、基质干扰小、图谱简单易于解析,检出限低一个数量级以上,在分析低含量、复杂基质的样品时更具优势。 相似文献
9.
10.
《Journal of separation science》2003,26(5):369-375
In a study aiming to characterize cork off‐flavour for quality control purposes, chloroanisoles were extracted and identified from cork stoppers by means of solid‐phase microextraction (SPME)–gas chromatography–ion‐trap mass spectrometry (GC–ITMS). An experimental design procedure was used to investigate the effects of some experimental parameters on the SPME of 2,4‐dichloroanisole, 2,6‐dichloroanisole, and 2,4,6‐trichloroanisole from cork stoppers by using a Carboxen‐PDMS 75 μm fibre. Variables such as extraction temperature, extraction time, and percentage of ethanol added to the matrix were optimized to improve extraction efficiency of chloroanisoles onto SPME fibre. Instrumental analysis was performed by GC–ITMS in the MS/MS mode. Preliminary analyses on standard solutions allowed selection of the appropriate ionization mode (i. e. electron impact or chemical ionization), providing for each analyte the highest instrumental response. In order to find polynomial functions describing the relationships between variables and responses, the analytical responses, i.e. the chromatographic peak areas, were processed by using the backward multiple regression analysis. For all the analytes the operating conditions providing the highest extraction yield inside the experimental domain considered were found. 相似文献
11.
Watcharaporn Hoisang Duangjai Nacapricha Prapin Wilairat Warawut Tiyapongpattana 《Journal of separation science》2019,42(11):2032-2043
Liquid microextraction employing solidification of the floating organic droplet, with vortexing and heating to optimize extraction efficiency, was developed for the determination of seven insecticides in fruit juice, vegetables, and agricultural runoff water. The extracts were analyzed by gas chromatography with both flame ionization and mass spectrometry detection for the determination of chlorpyrifos, prothiofos, profenofos, ethion, λ‐cyhalothrin, permethrin, and cypermethrin, respectively. Using 20 μL of 1‐undecanol in 10 mL of aqueous solution containing 1% w/v sodium chloride provided preconcentration factor of 500. The enrichment factor of the analytes was in the range of 355 to 509 with extraction recovery >71%. The linearity ranges were 4–200 μg/kg for gas chromatography with flame ionization detection and 1–100 μg/kg for gas chromatography with mass spectrometry, with limits of detection ranging from 0.04 to 1.2 μg/kg, which are lower than the international maximum residue limits for vegetables and fruit juice. Intra‐day and inter‐day precisions are less than 5.4 and 7.0% relative standard deviation, respectively. The method was successfully applied to the determination of the seven insecticides in samples of vegetables, fruit juice and agricultural runoff, with recoveries ranging from 61.7 to 120.8%. The extraction method is simple, efficient and environmentally friendly. 相似文献
12.
Fast gas chromatography with solid phase extraction clean-up for ultratrace analysis of pesticide residues in baby food 总被引:5,自引:0,他引:5
Hercegová A Dömötörová M Matisová E Kirchner M Otrekala R Stefuca V 《Journal of chromatography. A》2005,1084(1-2):46-53
A sample preparation method based on single solvent phase extraction and solid-phase extraction (SPE-NH2) clean-up is studied in combination with fast capillary gas chromatography (GC) to determine 18 selected pesticides belonging to various chemical classes in apples, the common raw material for baby food production and baby food, at the concentration level < or = 10 microg/kg maximum residual limit (MRL). Possibilities of mass spectrometry (MS) detector and electron capture detector (ECD) in fast gas chromatography (GC) of samples with complex matrice at ultra trace levels of pesticide residues were studied and compared. MS detection in single ion monitoring (SIM) mode provided higher selectivity compared to ECD. Optimisation of extraction as well as the simplifying of the whole process of sample preparation was carried out. Recoveries obtained at concentration level of 5 microg/kg (the required value for limit of quantification (LOQ) in baby food) were >90%, except of dimethoate (77.7%) and captan (46.4%) with MS detection. The obtained LOQs were at least 1 order lower than 5 microg/kg for the majority of compounds. The repeatability of gas chromatography-mass spectrometry (GC-MS) measurements of the matrix matched standards expressed as relative standard deviation was <11% except of captan and cypermethrin. 相似文献
13.
A supported liquid extraction LC–MS/MS method for determination of concentrations of GDC‐0425, a small molecule Checkpoint kinase 1 inhibitor,in human plasma
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Xiao Ding Yuan Chen Srikumar Sahasranaman Yifan Shi Janine McKnight Brian Dean 《Biomedical chromatography : BMC》2016,30(12):1984-1991
A liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for the determination of GDC‐0425 concentrations in human plasma has been developed and validated. Supported liquid extraction was used to extract plasma samples (50 μL) and the resulting samples were analyzed using reverse‐phase chromatography and mass spectrometry coupled with a turbo‐ionspray interface. The mass analysis of GDC‐0425 was performed using multiple reaction monitoring transitions in positive ionization mode. The method was validated over the calibration curve range of 1.00–1000 ng/mL using linear regression and 1/x2 weighting. Within‐run relative standard deviation ranged from 0.8 to 5.1%, while between‐run RSD varied from 1.9 to 4.7% for QCs. The accuracy ranged from 90.0 to 101.0% of nominal for within‐run and from 94.0 to 100.0% of nominal for between‐run. Overall extraction recovery was 87.4% for GDC‐0425 and 87.9% for GDC‐0425‐d9. Stability of GDC‐0425 was established in human plasma for 374 days at ?20 and ?70 °C and established in reconstituted sample extracts for 88 h when stored at 2–8 °C. Stable‐labeled internal standard was used to minimize matrix effects. This assay was used to characterize the pharmacokinetics of GDC‐0425 in cancer patients. 相似文献
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Jiping Huo Hongyun Wang Pei Hu Pingya Li Jinping Liu Ji Jiang 《Biomedical chromatography : BMC》2013,27(12):1701-1707
A specific, sensitive and rapid method based on high performance liquid chromatography coupled to tandem mass spectrometry (HPLC‐MS/MS) was developed for the determination of pseudo‐ginsenoside GQ in human plasma. Liquid–liquid extraction was used to isolate the analyte from biological matrix followed by injection of the extracts onto a C8 column with isocratic elution. Detection was carried out on a triple quadrupole tandem mass spectrometer (API‐4000 system) in multiple reaction monitoring mode using negative electrospray ionization. The mobile phase consisted of methanol–10 mm ammonium acetate (90:10, v/v) and the flow rate was 0.3 mL/min. The method was validated over the concentration range of 5.0–5000.0 ng/mL for plasma. Inter‐ and intra‐day precisions (relative standard deviation) were all within 15% and the accuracy (relative error) was ≤9.4%. The lower limit of quantitation was 5.0 ng/mL. The pseudo‐ginsenoside GQ was stable after 8 h at room temperature, 24 h at autosampler and three freeze–thaw cycles (from ?30 to 25 °C). The method was successfully applied to the pharmacokinetic study of pseudo‐ginsenoside GQ in healthy Chinese volunteers. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
17.
A. Ghassempour Mohammad Reza Arshadi Feridoun Salek Asghari 《Analytical and bioanalytical chemistry》2001,369(2):176-183
N-1-Naphthylphtalamic acid (naptalam) and its degradation products, 1-naphthylamine and N-(1-naphthyl) phthalimide were simultaneously determined in river water by two independent mass spectrometric (MS) methods. These were negative ion MS (NIMS) and programmable temperature vaporizer gas chromatography mass spectrometry (PTV-GC MS) with electron impact ionization (positive ions). Prior to the NIMS analysis, the samples were preconcentrated by solid phase extraction (SPE) of C18 membrane discs. The PTV-GC MS studies were performed without any preconcentration procedure. Selected ion monitoring (SIM) and internal standardization with naphthalene were applied in both methods. The limits of determination (LOD) of NIMS studies were 230, 270 and 260 ng L–1 for naptalam, 1-naphthylamine and N-(1-naphthyl) phthalimide, respectively, with relative standard deviation (RSD) < 1% (n = 5) and of PTV-GC MS 17, 11 and 15?ng L–1 (RSD < 0.7%, n = 5). The LOD, linearity, RSD and time required for these methods are far better than for HPLC analyses. 相似文献
18.
A quantitative method consisting of solid-phase extraction (SPE) followed by liquid chromatography/electrospray ionization ion trap mass spectrometry (LC/ESI-ITMS) analysis was developed for the identification and quantitation of ten pyrethroid pesticides commonly used in vegetables. The best HPLC separation was achieved using a gradient program of methanol/water mixture. For the vegetable samples, an SPE procedure to clean up the matrices was carried out prior to LC/MS analysis. Under the optimum conditions, the limits of quantification of the pyrethroid pesticides (tetramethrin, allethrin, fenpropathrin, lambda-cyhalothrin, cypermethrin, deltamethrin, fenvalerate, bioresmethrin, permethrin and bifenthrin) ranged from 0.03 to 0.1 mg kg-1 with relative standard deviations<20%, and the mean recoveries ranged from 69.5 to 102.5%. The proposed method has been successfully applied to the determination of pyrethroids in six vegetables with satisfactory results. 相似文献
19.
采用改进的分散固相萃取(QuEchERs)法对样品进行前处理,建立水果和蔬菜中毒杀芬残留的气相色谱–负化学电离源质谱(GC–NCI–MS)检测方法。样品中的毒杀芬由正己烷提取,经吸附剂PSA+GCB净化,在GC–NCI–MS的选择离子扫描模式下进样分析。毒杀芬的色谱保留时间在12.5~18.0 min区间内,采用面积归一化法积分,外标法定量。毒杀芬质量浓度在0.050~2.000 mg/L范围内与色谱峰面积呈良好的线性关系,相关系数r=0.999 1。分别以蓝莓、黄桃、菠菜为基质,在0.025,0.050 mg/kg添加水平下,毒杀芬的回收率为107.2%~118.1%,测定结果的相对标准偏差为5.5%~8.8%(n=6),定量限为0.025 mg/kg。该方法检测快速,适用于水果和蔬菜中毒杀芬残留的日常检测。 相似文献
20.
建立了超高效液相色谱―串联质谱/质谱法(HPLC-MS/MS)同时测定水质中诺氟沙星和氧氟沙星的分析方法。试样经HLB柱净化和C18柱分离,采用电喷雾离子源(ESI),正离子扫描,多反应监测(MRM)模式进行检测,外标法定量。结果表明,诺氟沙星和氧氟沙星在2~100?g/L浓度范围内线性关系良好,空白样品加标回收率均大于85%,相对标准偏差小于10%,诺氟沙星和氧氟沙星方法检出限(LOD)均为0.5 ng/m L,定量限为2 ng/m L。该方法准确、灵敏、操作相对简便,适用于同时测定水质中诺氟沙星和氧氟沙星。 相似文献