共查询到20条相似文献,搜索用时 15 毫秒
1.
The new analytical method using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedure for simultaneous determination
of diacylhydrazine insecticide residues in fruits and vegetables was developed using ultra-performance liquid chromatography
coupled with tandem mass spectrometry (UPLC-MS/MS). The four insecticides (tebufenozide, methoxfenozide, chromafenozide, and
halofenozide) were extracted from six fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary
secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to UPLC-MS/MS analysis. The determination of the target compounds
was achieved in less than 3.0 min using an electrospray ionization source in positive mode (ESI+) for tebufenozide, methoxfenozide,
and halofenozide and in negative mode (ESI−) for chromafenozide. The limits of detection were below 0.6 μg kg−1, while the limit of quantification did not exceed 2 μg kg−1 in different matrices. The QuEChERS procedure by using two sorbents (PSA and C18) and the matrix-matched standards gave satisfactory
recoveries and relative standard deviation (RSD) values in different matrices at four spiked levels (0.01, 0.05, 0.1, and
1 mg kg−1). The overall average recoveries for this method in apple, grape, cucumber, tomato, cabbage, and spinach at four levels ranged
from 74.2% to 112.5% with RSDs in the range of 1.4–13.8% (n = 5) for all analytes. This study provides a theoretical basis for China to draw up maximum residue limits and analytical
method for diacylhydrazine insecticide in vegetables and fruits. 相似文献
2.
This paper reports a novel approach for the detection, confirmation, and quantification of 15 selected pyrethroid pesticides,
including pyrethins, and two metabolites of dithiocarbamates in foods by ultra-performance liquid chromatography–tandem mass
spectrometry (UPLC–MS–MS). The proposed method makes use of a modified QuEChERS (quick, easy, cheap, effective, rugged, and
safe) procedure that combines isolation of the pesticides and sample cleanup in a single step. Analysis of pyrethroids and
dithiocarbamate metabolites was performed by UPLC–MS–MS operated with electrospray and atmospheric pressure chemical ionization,
respectively. Two specific precursor–product ion transitions were acquired per target compound in multiple reaction monitoring
(MRM) mode. Such acquisition achieved the minimum number of identification points according to European Commission (EC) document
no. SANCO/10684/2009, thus fulfilling the EC point system requirement for identification of contaminants in samples. The method
was validated with a variety of food samples. Calibration curves were linear and covered from 1 to 800 μg kg−1 in the sample for all target compounds. Average recoveries, measured at mass fractions of 10 and 100 μg kg−1 for pyrethroids and 5 and 50 μg kg−1 for dithiocarbamate metabolites, were in the range of 70–120% for all target compounds with relative standard deviations
below 20%. Method limits of quantification (MLOQ) were 10 μg kg−1 and 5 μg kg−1 for pyrethroids and dithiocarbamate metabolites, respectively. The method has been successfully applied to the analysis of
600 food samples in the course of the first Hong Kong total diet study with pyrethroids and metabolites of dithiocarbamates
being the pesticides determined. 相似文献
3.
M. V. Russo 《Chromatographia》2000,51(1-2):71-76
Summary A rapid method for the determination of chlorinated pesticides and polychlorinated biphenyls in mussels (Mytilus sp.) is reported.
The mussel sample is homogenized and extracted with acetonitrile. The organic solution is concentrated and successively diluted
with distilled water solution (12 g L−1 NaCl). The organic compounds from water solution are adsorbed onto a NH2 Sep-Pak cartridge.
The clean-up step, in which the polychlorobiphenyls and chiorinated pesticides are separated in different eluates, is achieved
by passing 25 mL of a 40% methanol aqueous solution through the NH2 Sep-Pak and the C18 Sep-Pak cartridges connected in series.
The polychloroblphenyls are desorbed from the NH2 Sep-Pak cartridge whilst the chlorinated peslicides are recovered from the C18 Sep-Pak cartridge.
In the separation of polychlorobiphenyls from the chlorinated pesticides tested in this work, only aldrin, hepatachlor and
4,4′-DDD are partially adsorbed with the polychlorobiphenyls onto the NH2 Sep-Pak cartridge.
The average recovery is ≥95.0% with a relative standard deviation ≤5.0%. The limits of detection for different pesticides
and polychlorobiphenyl congeners are 0.01 and 0.008 μg Kg−1. The final determination is carried out by capillary gas chromatography with ECD. 相似文献
4.
Summary Two procedures, based on large-volume injection with a programmed-temperature vaporizer (PTV), have been developed for the
determination of several triazine and organophosphorus pesticides. The use of PTV for injection in gas chromatography (GC)
has enabled the introduction of up to 200 μL sample extract into the GC, thus increasing the sensitivity of the method. PTV
injection has been combined off-line with two different microextraction procedures—liquid-liquid partition and solid-phase
extraction.
A simple and rapid off-line liquid-liquid microextraction procedure (5 mL water/1 mL methyltert-butyl ether) was applied to surface water samples spiked at levels between 0.01 and 5μg L−1. Recoveries of the overall procedure were >80% and the precision was better than 15%. Detection limits were <30 ngL−1 from 200-μL injections in GC-NPD analysis of triazines and GC-FPD analysis of organophosphorus pesticides. Off-line automated
solid-phase extraction with C18 cartridges has been applied to water samples (50 mL) spiked at 0.01, 0.1 and 1 μg L−1. The overall procedure was satisfactory (recoveries >80% and coefficients of variation <12%) and the limits of detection
ranged from 1 to 9 ng L−1.
Finally, several surface water samples were anlysed, and triazine herbicides were detected at concentrations of approx. 0.1–0.2
μg L−1. The results were similar to those obtained by conventional solvent extraction then GC-MSD after splitless injection of 2
μL. 相似文献
5.
Pérez-Ruiz T Martínez-Lozano C Martín J García MD 《Analytical and bioanalytical chemistry》2006,384(1):280-285
A very simple, rapid and highly sensitive flow injection fluorimetric method was developed for the determination of phylloquinone.
The assay was based on the on-line reduction of phylloquinone in dodecylsulfate micelles after irradiation with UV light.
The micellar medium enhanced the fluorescence and stability of the reduced phylloquinone. Under optimum experimental conditions,
the range of application of the technique was between 0.09 and 45.0 μg mL−1 and the detection limit was 0.05 μg mL−1. The sample throughput was 90 injections per hour. The reliability of the method for the routine analysis of phylloquinone
in vegetables and fruits is demonstrated. Extractions were made with hexane, and an automated solid phase extraction system
was used to purify the sample extracts prior to injection into the flow injection manifold. 相似文献
6.
Ion-exclusion chromatography (IEC) coupled with electrospray ionization quadrupole mass spectrometry (ESI-MS) has been used
for the analysis of carboxylic acids. The use of ESI-MS provides increased specificity and sensitivity compared to existing
detection methods. This paper applies IEC-ESI-MS to the analysis of carboxylic acids in commonly found root exudates and shows
that the separation of nine carboxylic acids (pyruvic, oxalic, lactic, malonic, maleic, succinic, tartaric, aconitic and citric
acids) can be achieved by IEC within 8 min. The ESI provided reasonable signals from negative ions, [M−H]− in the negative ionization mode. Linear plots of peak area versus concentration were obtained in the range 50–25,000 μg L−1 for MS detection under optimized MS conditions. The detection limits of target organic acids, based upon signal to noise
ratio (S/N = 3), ranged from 10 to 30 μg L−1. The reproducibility of peak areas was <2.5% (n = 5). The proposed method was used for the confirmation and quantification of carboxylic acids in nutrient solutions containing
root exudates. 相似文献
7.
Capillary zone electrophoresis determination of oxytetracycline in pig tissue samples at maximum residue limits 总被引:2,自引:0,他引:2
Summary The determination of the antibiotic oxytetracycline (OTC), in pig tissues was investigated by capillary zone electrophoresis
(CZE) with a prior solid-phase extraction (SPE) using alkyl-bonded silica and polymeric cartridges. The methodology developed
allows determination of OTC in pig kidney, liver and muscle samples with detection limits below maximum residue limit values,
and the procedures to extract OTC and clean-up the matrix are simple and reliable. The limit of detection for OTC was 160,
120 and 85 μg kg−1 for kidney, liver and muscle samples, respectively. The average recoveries from spiked samples (200 μg kg−1 and 1600 μg kg−1) were in excess of 63% with coefficients of variation between 2.0 and 9.8%. This method would be useful for routine monitoring
of oxytetracycline residues in pig tissues. 相似文献
8.
Delhomme O Raeppel C Teigné D Briand O Millet M 《Analytical and bioanalytical chemistry》2011,399(3):1325-1334
To measure dermal exposure of a non-agricultural occupationally exposed population to pesticides, a new method has been developed
for analysis of 13 pesticides from different classes (fungicides, herbicides, insecticides) on dermal patches. The method
includes extraction of the patches and analysis of the pesticides by GC–MS and/or HPLC–fluorescence. Water-soluble pesticides
(glyphosate and glufosinate) on patches were ultrasonically extracted twice with ultra-pure water for 10 min and analysed
by HPLC–fluorescence after derivatisation with FMOC. Organic-soluble pesticides (bifenthrin, cyprodinil, difufenicanil, fludioxonil,
oxadiazon, pyriproxyfen, clopyralid, 2,4-D, fluroxypyr, 2,4-MCPA, and triclopyr) were extracted ultrasonically twice for 10 min
with 70:30 dichloromethane–acetonitrile and analysed by GC–MS directly or after derivatisation with N-methyl-N-tert-butyldimethylsilyltrifluoroacetamide. Detection limits varied between 3 and 4 μg L−1 for water-soluble pesticides and between 1 and 10 μg L−1 for organic-soluble pesticides. 相似文献
9.
Carvalho JJ Jerónimo PC Gonçalves C Alpendurada MF 《Analytical and bioanalytical chemistry》2008,392(5):955-968
European Council Directive 98/83/EC on the quality of water intended for human consumption brought a new challenge for water-quality
control routine laboratories, mainly on pesticides analysis. Under the guidelines of ISO/IEC 17025:2005, a multiresidue method
was developed, validated, implemented in routine, and studied with real samples during a one-year period. The proposed method
enables routine laboratories to handle a large number of samples, since 28 pesticides of 14 different chemical groups can
be quantitated in a single procedure. The method comprises a solid-phase extraction step and subsequent analysis by liquid
chromatography-mass spectrometry (LC-MS-MS). The accuracy was established on the basis of participation in interlaboratory
proficiency tests, with encouraging results (majority |z-score| <2), and the precision was consistently analysed over one year. The limits of quantitation (below 0.050 μg L−1) are in agreement with the enforced threshold value for pesticides of 0.10 μg L−1. Overall method performance is suitable for routine use according to accreditation rules, taking into account the data collected
over one year.
Figure Simultaneous SPE extraction system for high thoughput analysis
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.
Notes: IAREN is an accredited laboratory under the ISO/IEC 17025:2005 for 165 analytical determinations and part of the NORMAN
Network of Reference laboratories for monitoring of emerging environmental pollutants in the European Union.
This work was presented (podium presentation) at the 12th Symposium on Sampling and Handling of the International Association
of Environmental Analytical Chemistry (IAEAC), Zaragoza, 2006. 相似文献
10.
Liu X Xu J Li Y Dong F Li J Song W Zheng Y 《Analytical and bioanalytical chemistry》2011,399(7):2539-2547
A sensitive and effective method for simultaneous determination of triazolopyrimidine sulfonamide herbicide residues in soil,
water, and wheat was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry. The four
herbicides (pyroxsulam, flumetsulam, metosulam, and diclosulam) were cleaned up with an off-line C18 SPE cartridge and detected
by tandem mass spectrometry using an electrospray ionization source in positive mode (ESI+). The determination of the target
compounds was achieved in <2.0 min. The limits of detection were below 1 μg kg−1, while the limits of quantification did not exceed 3 μg kg−1 in different matrices. Quantitation was determined from calibration curves of standards containing 0.05–100 μg L−1 with r
2 > 0.997. Recovery studies were conducted at three spiked levels (0.2, 1, and 5 μg kg−1 for water; 5, 10, and 100 μg kg−1 for soil and wheat). The overall average recoveries for this method in water, soil, wheat plants, and seeds at three levels
ranged from 75.4% to 106.0%, with relative standard deviations in the range of 2.1–12.5% (n = 5) for all analytes. 相似文献
11.
Mol HG Rooseboom A van Dam R Roding M Arondeus K Sunarto S 《Analytical and bioanalytical chemistry》2007,389(6):1715-1754
The ethyl acetate-based multi-residue method for determination of pesticide residues in produce has been modified for gas
chromatographic (GC) analysis by implementation of dispersive solid-phase extraction (using primary–secondary amine and graphitized
carbon black) and large-volume (20 μL) injection. The same extract, before clean-up and after a change of solvent, was also
analyzed by liquid chromatography with tandem mass spectrometry (LC–MS–MS). All aspects related to sample preparation were
re-assessed with regard to ease and speed of the analysis. The principle of the extraction procedure (solvent, salt) was not
changed, to avoid the possibility invalidating data acquired over past decades. The modifications were made with techniques
currently commonly applied in routine laboratories, GC–MS and LC–MS–MS, in mind. The modified method enables processing (from
homogenization until final extracts for both GC and LC) of 30 samples per eight hours per person. Limits of quantification
(LOQs) of 0.01 mg kg−1 were achieved with both GC–MS (full-scan acquisition, 10 mg matrix equivalent injected) and LC–MS–MS (2 mg injected) for
most of the pesticides. Validation data for 341 pesticides and degradation products are presented. A compilation of analytical
quality-control data for pesticides routinely analyzed by GC–MS (135 compounds) and LC–MS–MS (136 compounds) in over 100 different
matrices, obtained over a period of 15 months, are also presented and discussed. At the 0.05 mg kg−1 level acceptable recoveries were obtained for 93% (GC–MS) and 92% (LC–MS–MS) of pesticide–matrix combinations. 相似文献
12.
A confirmatory and quantitative method based on liquid chromatography–electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS)
has been developed for simultaneous determination of seven photoinitiator residues: benzophenone, (1-hydroxycyclohexyl)phenylketone
(Irgacure 184), isopropylthioxanthone (ITX), 2-ethylhexyl-(4-dimethylamino)benzoate (EHA or EHDAB), 2-methyl-1-[4-(methylthio)phenyl]-2-(4-morpholinyl)-1-propanone
(Irgacure 907), (2,4,6-trimethylbenzoyl)diphenylphosphine oxide (TPO) and 2-benzyl-2-(dimethylamino)-1-(4-morpholinophenyl)-1-butanone
(Irgacure 369) in packaged milk and related packaging materials. Residues of photoinitiators were extracted from milk using
acetonitrile, and further enriched and purified on HLB solid-phase extraction cartridges prior to being analyzed by LC-ESI/MS/MS
with selected reaction monitoring mode, while photoinitiators in packaging materials were extracted using the same solvent.
Satisfactory recovery (from 80 to 111%), intra- and inter-day precision (below 12%), and low limits of quantification (from
0.1 to 5.0 μg kg−1) were evaluated from spiked samples at three concentration levels (5.0, 10.0 and 25.0 μg kg−1 for Irgacure 184 and 2.5, 5.0 and 25.0 μg kg−1 for others). These excellent validation data suggested the possibility of using the LC-ESI/MS/MS method for simultaneous
determination of low-level photoinitiator residues migrating from printed food-packaging materials into milk. The method has
been successfully applied to the analysis of real samples of different fat contents ranging from 8 to 30 g L−1. The photoinitiator residues were revealed to be higher in milk with higher fat content and the most important contaminations
were benzophenone and ITX in concentration ranges of 2.84–18.35 and 0.83–8.87 μg kg−1, respectively. 相似文献
13.
Summary Gas chromatography of polychlorinated biphenyls and chlorinated pesticides in water samples is carried out after adsorption
from a 25–500 mL sample, on a cartridge containing 100 mg aminopropyl-bonded porous silica. The clean-up step in which the
PCBs and chlorinated pesticides are separated in different eluates is achieved by passing 25 mL of 40% aqueous methanol through
the NH2 Sep-Pak cartridge. The PCBs are desorbed with 500 μL ethylacetate, which is concentrated and analysis by GC-ECD. The average
recovery, at 1 ppb is >97% with a standard deviation <2. The limits of detection are 0.1 ng μL−1 and 5 pg μL−1 respectively for Cl3-PCB and Cl8-PCB congeners. In the separation of PCBs from the chlorinated pesticides tested in this work, only the Aldrin is adsorbed
for 60% with the PCBs by the NH2 Sep-Pak cartridge. The method described is rapid, simple and reproducible. 相似文献
14.
E. W. J. Hooijschuur Ch. E. Kientz J. Dijksman U. A. Th. Brinkman 《Chromatographia》2001,54(5-6):295-301
Summary The potential of microcolumn liquid chromatography (μlC) and capillary electrophoresis (CE) with on-line, flame photometric
detection (FPD) in the P-selective mode has been studied for determination of polar P-containing pesticides, glyphosate and
its main metabolite, aminomethylphosphonic acid (AMPA), ethephon, fosetyl-aluminium and acephate. Acephate was determined
by reversed-phase μLLC-FPD using large-volume injections with peak compression, the other compounds were determined by μLC-FPD
and CE-FPD using simple, large-volume injection procedures to obtain limits of detection of 7.5-500 ng·mL−1 and 1.0 μ·mL−1, respectively. The methods showed acceptable repeatability and robustness and were successfully applied for rapid and selective
determination of pesticides in fruit, vegetable and water samples. 相似文献
15.
To determine sulphamethazine (SMZ) residues in edible animal foods (pig muscle, chicken muscle, egg, fish, milk and liver),
a competitive direct enzyme-linked immunosorbent assay (ELISA) and a colloidal gold immunoassay were established. The limits
of detection of the ELISA and the colloidal gold immunoassay were 0.02 and 0.5 μg kg−1, respectively. The specificity of the ELISA developed to the SMZ was high according to the results of cross-reactivity testing
with 14 kinds of sulphonamides. To obtain a more sensitive immunoassay, buffer solution (30 mmol L−1 phosphate-buffered saline with 0.05% Tween 20, pH 8.5) was optimized through the whole test procedure. A simple and efficient
extraction method for the rapid detection of SMZ residues in foods was developed, with recoveries between 74 and 117.5%. Matrix
effects can be avoided by 1:10 dilution of pig muscle, chicken muscle, egg, fish, milk and liver with optimal buffer. The
detection limit of SMZ was 5 μg kg−1 in liver and 2 μg kg−1 in the other five samples. For the validation of the ELISA tests, sample extracts were analysed by ELISA and high-performance
liquid chromatography. The results obtained by these two methods showed a good correlation (r
2) which was greater than 0.9. The colloidal gold immunoassay presented in this assay was successfully applied to determine
SMZ in pig muscle, milk and fish below or equal to the maximum residue level (20 μg kg−1). 相似文献
16.
Dolores Barranco Martínez María Martínez Galera Piedad Parrilla Vázquez M. Dolores Gil García 《Chromatographia》2007,66(7-8):533-538
Liquid chromatography with electrospray mass spectrometry (LC–ESI-MS) instrumentation equipped with a single quadrupole mass
filter has been used to determine several benzoylphenylurea insecticides (diflubenzuron, triflumuron, hexaflumuron, lufenuron
and flufenoxuron). Chromatographic and MS parameters were optimised to obtain the best sensitivity and selectivity for all
pesticides. Solid-phase extraction (SPE) using C18 cartridges was applied for preconcentration of pesticide trace levels in river water samples. Recoveries of benzoylphenylurea
pesticides from spiked river water (0.01 and 0.025 μg L−1) were between 73 and 110% and detection limits were between 3.5 and 7.5 ng L−1. The applicability of the method to the determination of benzoylphenylurea insecticides in spiked cucumber, green beans,
tomatoes and aubergines was evaluated. Samples were extracted into dichloromethane without any clean-up step. The limits of
detection ranged from 1.0 to 3.2 ng mL−1 (0.68 and 2.13 μg kg−1 in the vegetable samples). Mean recoveries ranged from 79 to 114% at spiking levels of 0.01 and 0.03 mg kg−1. The method was applied to determine traces of benzoylphenylureas in both river water and vegetable samples with precision
values lower than 10%. Interferences due to the matrix effect were overcome using matrix-matched standards. 相似文献
17.
Martínez-Uroz MA Mezcua M Belmonte Valles N Fernández-Alba AR 《Analytical and bioanalytical chemistry》2012,402(3):1365-1372
A gas chromatography–mass spectrometry method in negative chemical ionization mode has been developed incorporating simultaneous
detection using a micro-electron capture detector (μ-ECD) for the determination of pesticides in fruits and vegetables. This
instrument configuration uses a three-way splitter device which divides the effluent from the analytical column between the
two detectors with the split ratio 1:0.1 (MSD/μ-ECD) in each run. The μ-ECD was used for confirmation purposes. Validation
of the method was performed on three matrices: tomato, apple, and orange. The ethyl acetate method was assayed; recovery studies
were performed at 10 and 100 μg/kg. Recoveries between 70% and 120% were achieved and relative standard deviations lower than
20% (n = 5) were obtained for all pesticides and matrices studied. Limits of quantification lower than 10 μg/kg were obtained for
100% of pesticides in all of the matrices. Limits of quantification lower than 2.5 μg/kg were achieved for 77.8% of pesticides
in the tomato and apple matrices, and for 72.2% of pesticides in the orange matrix. The method showed linear response in the
concentration range tested (2.5–500 μg/kg) with correlation coefficients >0.99. Good repeatability and reproducibility results
were obtained in all cases, with relative standard deviations lower than 16.7% and 20%, respectively. Finally, 20 incurred
samples were analyzed using the proposed method. The simultaneous use of the two detectors was satisfactory for the analysis
of these real samples. The total number of pesticides identified was 25. The number of samples which contained at least one
pesticide was 15—this represented 75% of the total number of samples studied. 相似文献
18.
Herranz S Ramón-Azcón J Benito-Peña E Marazuela MD Marco MP Moreno-Bondi MC 《Analytical and bioanalytical chemistry》2008,391(5):1801-1812
Specific polyclonal antibodies against s-triazine herbicides were obtained by preparing immunogens coupling home-synthesized haptens derivatives of simazine (6-chloro-N-ethyl-N′-ethyl-1,3,5-triazine-2,4-diamine) to lysine groups of hemocyanin from keyhole limpets and bovine serum albumin carrier proteins.
Three highly sensitive rabbit antisera were obtained and evaluated with a battery of six enzyme tracers derived from triazine
structures in an optimized ELISA format. The antiserum As8 and the HRP-2f tracer, which yield the best assay sensitivity for
simazine (detection limit 0.11 ± 0.02 μg L−1, IC50 0.88 ± 0.04 μg L−1), were applied to the development of a sensitive flow-through immunoassay for the analysis of this herbicide. The automated
assay was based on a direct competitive immunosorbent assay and fluorescence detection. The optimized method presents an IC50 value of 0.35 ± 0.04 μg L−1 with a detection limit of 1.3 ± 0.9 ng L−1 and a dynamic range from 0.010 to 7.5 μg L−1 simazine. The generic nature of the antiserum was shown by good relative cross-reactivities with other triazines such as
atrazine (420%) or propazine (130%) and a lower response to terbutylazine (6.4%) and desethyl-atrazine (2.2%). No cross-reactivity
was obtained for nonrelated pesticides such as 2,4-dichlorophenoxyacetic acid or linuron and the assay could be applied as
a screening method for triazine herbicides. The total analysis time was 30 min per determination and the immunosensor could
be reused for more than 150 cycles without significant loss of activity. The immunosensor has been successfully applied to
the direct analysis of simazine in surface water samples at the nanogram per liter level. The results obtained by comparative
analysis of the immunosensor with a chromatographic procedure for triazines showed a close correspondence. 相似文献
19.
Determination of Organophosphorus Pesticides in Soil by MMSPD-GC-NPD and Confirmation by GC-MS 总被引:1,自引:0,他引:1
A novel method, modified matrix solid-phase dispersion (MMSPD), has been developed for quantitative analysis of organophosphorus
pesticide residues in soil. It was based on matrix solid-phase dispersion (MSPD) and continuous liquid-solid extraction (continuous
LSE), using Florisil as sorbent and dichloromethane as the recycling solvent. Two soils with different texture and physicochemical
properties were studied to validate the method. The effect of residence time of pesticides in soil was also studied. MMSPD
was compared with MSPD and continuous LSE respectively. Determination was carried out by gas chromatography with nitrogen-phosphorus
detection (GC-NPD). The method gave recoveries ranging from 72–105% with relative standard deviations (RSDs) lower than 15%
for the pesticides studied. The limits of detection (LODs) ranged from 0.1 to 0.6 ng g−1. Two pesticide residues have been detected in real soil samples from Fujian, China, using MMSPD. The pesticides were confirmed
by gas chromatography-mass spectrometry (GC-MS) in a selected-ion monitoring (SIM) mode.
Revised: 4 and 9 April 2006 相似文献
20.
Yan Liang Jie Sun Lin Xie An Kang Yuan Xie Wei-Dong Chen Hua Lv Guang-Ji Wang 《Chromatographia》2007,66(3-4):165-170
A sensitive and specific liquid chromatographic method with electrospray ionization mass spectrometry (LC–ESI-MS) has been
developed and validated for identification and quantification of mitiglinide in human urine. A simple liquid–liquid extraction
procedure was followed by separation on a C18 column with gradient elution, and detection using a single-quadrupole mass spectrometer in selected-ion-monitoring (SIM)
mode. The method was tested using six different batches of urine. Linearity was established for the mitiglinide concentrations
in the range 0.005–1.0 μg mL−1, with a coefficient of determination (r) of 0.9998 and good back-calculated accuracy and precision. Intra- and inter-day precision (as RSD, %) was below 10% and
accuracy for mitiglinide ranged from 85 to 115%. The lower limit of quantification was reproducible at 0.002 μg mL−1 for 500 μL urine. The proposed method enables unambiguous identification and quantification of mitiglinide in pre-clinical
and clinical studies. 相似文献