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1.
Numata M Yarita T Aoyagi Y Tsuda Y Yamazaki M Takatsu A Ishikawa K Chiba K Okamaoto K 《Analytical and bioanalytical chemistry》2007,387(7):2313-2323
Two marine sediment certified reference materials, NMIJ CRM 7304-a and 7305-a, have been issued by the National Metrology
Institute of Japan in the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST) for the determination
of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs). The raw materials of the CRMs were collected from
a bay near industrial activity in Japan. Characterization of these CRMs was conducted by NMIJ, where the sediments were analyzed
using multiple analytical methods such as pressurized liquid extraction (PLE), microwave-assisted extraction (MAE), saponification,
Soxhlet extraction, supercritical fluid extraction (SFE), and ultrasonic extraction; the target compounds were determined
by one of the primary methods of measurements, isotope dilution–mass spectrometry (ID-MS). Certified values have been provided
for 14 PCB congeners (PCB numbers 3, 15, 28, 31, 70, 101, 105, 138, 153, 170, 180, 194, 206, 209) and 4 OCPs (γ-HCH, 4,4′-DDT,
4,4′-DDE, 4,4′-DDD) in both CRMs. NMIJ CRM 7304-a has concentrations of the contaminants that are a factor of 2–15 greater
than in CRM 7305-a. Both CRMs have information values for PCB homolog concentrations determined by collaborative analysis
using a Japanese official method for determination of PCBs. The total PCB concentrations in the CRMs are approximately 920
and 86 μg kg−1 dry mass respectively.
Electronic supplementary material Supplementary material is available in the online version of this article at and is accessible for authorized users. 相似文献
2.
Progesterone is one of the steroid hormones. The hormone is especially important in preparing the uterus for the implantation
of the blastocyst and in maintaining pregnancy. Its concentration in serum is measured to determine ovarian function and to
predict early pregnancy. The progesterone concentration is also important for in-vitro fertilization and embryo-transfer outcomes.
We have established isotope dilution liquid chromatography–tandem mass spectrometry as a primary method for the measurement
of progesterone in human serum. Progesterone and its isotopic analogue, progesterone-13C2, in serum were monitored at mass transitions of m/z 315.2/109.2 and 317.2/111.2 respectively in multiple-reaction monitoring (MRM) mode with electrospray positive ionization.
For validation of the method, progesterone in a National Institute of Standards and Technology standard reference material
(NIST SRM) was measured, and the measured results were in good agreement with the reference values within the uncertainty.
On the basis of the established method, progesterone certified reference material (CRM) was developed in this work. The certified
value was (1.41 ± 0.036) μg kg−1. The repeatability of 1.1% and reproducibility of 0.14% showed that ID LC–MS–MS is a reliable and reproducible method. The
expanded uncertainty for the measurement of progesterone in the CRM was approximately 2.6% within 95% confidence limits. The
detection limit of progesterone was approximately 0.6 μg kg−1. The progesterone CRMs were distributed to representative clinical laboratories in the Republic of Korea for comparison with
the chemiluminescence immunoassay (CLIA), which is the most sensitive immunoassay method. The results from the comparison
showed quite a large bias among the participating laboratories. This implies that the CRM is a very important material for
establishment of traceability to its practical use. 相似文献
3.
José Luis Martínez Vidal Antonia Garrido Frenich María de las Nieves Barco Bonilla Roberto Romero-González Juan Antonio Padilla Sánchez 《Analytical and bioanalytical chemistry》2009,395(5):1551-1562
A simple and rapid method based on pressurized liquid extraction has been validated for the simultaneous extraction of polychlorinated
biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs) from agricultural soil samples. Effective extraction was carried
out in less than 17 min for all the studied compounds, and good recoveries were obtained for PAHs and PCBs, ranging from 70%
to 112%, when blank samples were spiked at 2.5 μg kg−1, except for naphthalene with recoveries close to 40%. The separation and determination were performed by gas chromatography
coupled to tandem mass spectrometry using a triple quadrupole mass analyzer. The target compounds were detected by electron
impact with selected reaction monitoring, and mass spectrometric conditions were optimized in order to increase selectivity
and sensitivity. The developed method was validated, and matrix-matched calibration was used for quantification purposes.
Repeatability and interday precision ranged from 0.9% to 16.8% and from 1.6% to 22.3%, respectively. Limits of quantification
ranged from 0.07 to 2.50 μg kg−1. The proposed method was applied to the analysis of agricultural soil samples collected from Almeria (Spain), and PAHs and
PCBs were detected in some samples at concentrations ranging from 0.1 to 210 μg kg−1. 相似文献
4.
Numata M Aoyagi Y Matsuo M Ishikawa K Hanari N Otsuka S Tsuda Y Yarita T 《Analytical and bioanalytical chemistry》2008,391(6):1985-1995
Four mineral oil certified reference materials (CRMs), NMIJ CRM 7902-a, CRM 7903-a, CRM 7904-a, and CRM 7905-a, have been
issued by the National Metrology Institute of Japan, which is part of the National Institute of Advanced Industrial Science
and Technology (NMIJ/AIST), for the determination of polychlorinated biphenyls (PCBs). The raw materials for the CRMs were
an insulation oil (CRM 7902-a and CRM 7903-a) and a fuel oil (CRM7904-a and CRM 7905-a). A solution of PCB3, PCB8, and technical
PCB products, comprising four types of Kaneclor, was added to the oil matrices. The total PCB concentrations in the PCB-fortified
oils (CRM 7902-a and CRM 7904-a) are approximately 6 mg kg−1. In addition, the mineral oils which were not fortified with PCBs were also distributed as CRMs (CRM 7903-a and CRM 7905-a).
Characterization of these CRMs was conducted by the NMIJ/AIST, where the mineral oils and the PCB solution were analyzed using
multiple analytical methods such as dimethylsulfoxide extraction, normal-phase liquid chromatography, gel permeation chromatography,
reversed-phase liquid chromatography, and chromatography using sulfoxide-bonded silica; and/or various capillary columns for
gas chromatography, and two ionization modes for mass spectrometry. The target compounds in the mineral oils and those in
the PCB solution were determined by one of the primary methods of measurement, isotope dilution–mass spectrometry (ID-MS).
Certified values have been provided for 11 PCB congeners (PCB3, 8, 28, 52, 101, 118, 138, 153, 180, 194, and 206) in the CRMs.
These CRMs have information values for PCB homologue concentrations determined by using a Japanese official method for determination
of PCBs in wastes and densities determined with an oscillational density meter. Because oil samples having arbitrary PCB concentrations
between respective property values of the PCB-fortified and nonfortified CRMs can be prepared by gravimetric mixing of the
CRM pairs, these CRMs can be used for validation of PCB analyses using various instruments which have different sensitivities.
Figure Preparation and certification processes of the mineral oil CRMs (example shown is polychlorinated biphenyls in insulation
oil, high/low concentrations)
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
5.
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
6.
Rabindra N. Roy Lakshmi N. Roy Shahaf Ashkenazi Joshua T. Wollen Craig D. Dunseth Michael S. Fuge Jared L. Durden Chandra N. Roy Hannah M. Hughes Brett T. Morris Kevin L. Cline 《Journal of solution chemistry》2009,38(4):449-458
The values of the second dissociation constant, pK
2, of N-(2-hydroxyethyl) piperazine-N′-2-ethanesulfonic acid (HEPES) have been reported at twelve temperatures over the temperature range 5 to 55 °C, including
37 °C. This paper reports the results for the pa
H of eight isotonic saline buffer solutions with an I=0.16 mol⋅kg−1 including compositions: (a) HEPES (0.01 mol⋅kg−1) + NaHEPES (0.01 mol⋅kg−1) + NaCl (0.15 mol⋅kg−1); (b) HEPES (0.02 mol⋅kg−1) + NaHEPES (0.02 mol⋅kg−1) + NaCl (0.14 mol⋅kg−1); (c) HEPES (0.03 mol⋅kg−1) + NaHEPES (0.03 mol⋅kg−1) + NaCl (0.13 mol⋅kg−1); (d) HEPES (0.04 mol⋅kg−1) + NaHEPES (0.04 mol⋅kg−1) + NaCl (0.12 mol⋅kg−1); (e) HEPES (0.05 mol⋅kg−1) + NaHEPES (0.05 mol⋅kg−1) + NaCl (0.11 mol⋅kg−1); (f) HEPES (0.06 mol⋅kg−1) + NaHEPES (0.06 mol⋅kg−1) + NaCl (0.10 mol⋅kg−1); (g) HEPES (0.07 mol⋅kg−1) + NaHEPES (0.07 mol⋅kg−1) + NaCl (0.09 mol⋅kg−1); and (h) HEPES (0.08 mol⋅kg−1) + NaHEPES (0.08 mol⋅kg−1) + NaCl (0.08 mol⋅kg−1). Conventional pa
H values, for all eight buffer solutions from 5 to 55 °C, have been calculated. The operational pH values with liquid junction
corrections, at 25 and 37 °C have been determined based on the NBS/NIST standard between the physiological phosphate standard
and four buffer solutions. These are recommended as pH standards for physiological fluids in the range of pH = 7.3 to 7.5
at I=0.16 mol⋅kg−1. 相似文献
7.
Certified reference material for quantification of polycyclic aromatic hydrocarbons in sediment from the National Metrology Institute of Japan 总被引:2,自引:0,他引:2
Nobuyasu Itoh Yoshie Aoyagi Akiko Takatsu Takashi Yarita 《Analytical and bioanalytical chemistry》2009,393(8):2039-2049
The National Metrology Institute of Japan has issued a certified reference material (CRM) of freshwater lake sediment for
polycyclic aromatic hydrocarbon (PAHs) analyses. The certification used three extraction techniques: pressurized liquid extraction
(PLE) with toluene, PLE with dichloromethane/ethyl acetate (1:1 by volume), and alkaline extraction (1 M KOH in methanol)
in combination with microwave-assisted extraction. Both gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/dopant-assisted
atmospheric pressure photoionization/MS (LC/DA-APPI/MS) analyses were used. Certified values are provided for 18 PAHs at 1–25 μg
kg−1 except for perylene (2.08 × 103 μg kg−1), and information values are provided for two. Since the values of PAHs in the CRM are much lower than those in other CRMs
and are comparable to those found at sites with little human influence, the CRM is suitable for PAH monitoring in sediment
and soil samples. 相似文献
8.
L. Giannetti F. Longo F. Buiarelli M. V. Russo B. Neri 《Analytical and bioanalytical chemistry》2010,398(2):1017-1023
A specific, sensitive and robust liquid chromatography tandem mass spectrometry method for determining oxytetracycline, tetracycline,
chlortetracycline and doxycycline in royal jelly and honey samples is presented. Extraction of drug residues was performed
by ammonium acetate buffer as extractant followed by a clean-up with metal chelate affinity chromatography and solid-phase
extraction. Tetracycline analysis was performed using liquid chromatography–electrospray ionisation–tandem mass spectrometry.
The presented method is the first validated for royal jelly and in accordance with the requirements set by Commission Decision
2002/657/EC. Recoveries of the methods, calculated spiking the samples at 5.0, 10.0, 20.0 and 30.0 μg kg−1, were 79% to 90% for honey and 77% to 90% for royal jelly. The intra-day precision (RSD) ranged between 8.1% and 15.0% for
honey and from 9.1% to 16.3% for royal jelly, while inter-day precision values were from 10.2% to 17.6% and from 10.6% to
18.4% respectively for honey and royal jelly. Linearity for the four analytes was calculated from 5.0 to 50.0 μg kg−1. The decision limits (CCα) ranged from 6.2 to 6.4 μg kg−1 and from 6.1 to 6.5 μg kg−1 for honey and royal jelly, respectively. Detection capabilities values (CCβ) ranged between 7.2 and 7.7 μg kg−1 and from 7.3 to 7.9 μg kg−1 respectively for honey and royal jelly. The developed method is currently in use for confirmation of the official control
analysis of honey and royal jelly samples. 相似文献
9.
Hossein Amani Mohammad Reza Mehrnia Mohammad Hossein Sarrafzadeh Manouchehr Haghighi Mohammad Reza Soudi 《Applied biochemistry and biotechnology》2010,162(2):510-523
There is a lack of fundamental knowledge about the scale up of biosurfactant production. In order to develop suitable technology
of commercialization, carrying out tests in shake flasks and bioreactors was essential. A reactor with integrated foam collector
was designed for biosurfactant production using Bacillus subtilis isolated from agricultural soil. The yield of biosurfactant on biomass (Y
p/x), biosurfactant on sucrose (Y
p/s), and the volumetric production rate (Y) for shake flask were obtained about 0.45 g g−1, 0.18 g g−1, and 0.03 g l−1 h−1, respectively. The best condition for bioreactor was 300 rpm and 1.5 vvm, giving Y
x/s, Y
p/x, Y
p/s, and Y of 0.42 g g−1, 0.595 g g−1, 0.25 g g−1, and 0.057 g l−1 h−1, respectively. The biosurfactant maximum production, 2.5 g l−1, was reached in 44 h of growth, which was 28% better than the shake flask. The obtained volumetric oxygen transfer coefficient
(K
L
a) values at optimum conditions in the shake flask and the bioreactor were found to be around 0.01 and 0.0117 s−1, respectively. Comparison of K
L
a values at optimum conditions shows that biosurfactant production scaling up from shake flask to bioreactor can be done with
K
L
a as scale up criterion very accurately. Nearly 8% of original oil in place was recovered using this biosurfactant after water
flooding in the sand pack. 相似文献
10.
Clémens S Monperrus M Donard OF Amouroux D Guérin T 《Analytical and bioanalytical chemistry》2011,401(9):2699-2711
Methylmercury (MeHg) and total mercury (THg) in seafood were determined using species-specific isotope dilution analysis and
gas chromatography combined with inductively coupled plasma mass spectrometry. Sample preparation methods (extraction and
derivation step) were evaluated on certified reference materials using isotopically enriched Hg species. Solid–liquid extraction,
derivation by propylation and automated agitation gave excellent accuracy and precision results. Satisfactory figures of merit
for the selected method were obtained in terms of limit of quantification (1.2 μg Hg kg−1 for MeHg and 1.4 μg Hg kg−1 for THg), repeatability (1.3–1.7%), intermediate precision reproducibility (1.5% for MeHg and 2.2% for THg) and trueness
(bias error less than 7%). By means of a recent strategy based on accuracy profiles (β-expectation tolerance intervals), the
selected method was successfully validated in the range of approximately 0.15–5.1 mg kg−1 for MeHg and 0.27–5.2 mg kg−1 for THg. Probability β was set to 95% and the acceptability limits to ±15%. The method was then applied to 62 seafood samples
representative of consumption in the French population. The MeHg concentrations were generally low (1.9–588 μg kg−1), and the percentage of MeHg varied from 28% to 98% in shellfish and from 84% to 97% in fish. For all real samples tested,
methylation and demethylation reactions were not significant, except in one oyster sample. The method presented here could
be used for monitoring food contamination by MeHg and inorganic Hg in the future to more accurately assess human exposure. 相似文献
11.
Zang X Wang J Wang O Wang M Ma J Xi G Wang Z 《Analytical and bioanalytical chemistry》2008,392(4):749-754
A novel method was developed for the determination of captan, folpet, and captafol in apples by dispersive liquid–liquid microextraction
(DLLME) coupled with gas chromatography–electron capture detection (GC–ECD). Some experimental parameters that influence the
extraction efficiency, such as the type and volume of the disperser solvents and extraction solvents, extraction time, and
addition of salt, were studied and optimized to obtain the best extraction results. Under the optimum conditions, high enrichment
factors for the compounds were achieved ranging from 824 to 912. The recoveries of fungicides in apples at spiking levels
of 20.0 μg kg−1 and 70.0 μg kg−1 were 93.0–109.5% and 95.4–107.7%, respectively. The relative standard deviations (RSDs) for the apple samples at 30.0 μg kg−1 of each fungicide were in the range from 3.8 to 4.9%. The limits of detection were between 3.0 and 8.0 μg kg−1. The linearity of the method ranged from 10 to 100 μg kg−1 for the three fungicides, with correlation coefficients (r
2) varying from 0.9982 to 0.9997. The obtained results show that the DLLME combined with GC–ECD can satisfy the requirements
for the determination of fungicides in apple samples.
Figure Dispersive liquid–liquid microextraction (DLLME) coupled with gas chromatography–electron capture detection (GC–ECD) allows
satisfactory determination of fungicides in apple samples 相似文献
12.
Frank Marken Alastair N. Blythe Jay D. Wadhawan Richard G. Compton Steven D. Bull Robin T. Aplin Stephen G. Davies 《Journal of Solid State Electrochemistry》2001,5(1):17-22
The effect of the structure of the organic precursor molecule on the electroinsertion of anions and on the formation of materials
in the ionic liquid state is compared for three compounds, para-N, N, N′, N′-tetrahexylphenylenediamine (p-THPD), meta-N, N, N′, N′-tetrahexylphenylene diamine (m-THPD), and para-N, N, N′, N′-tetrakis(6-methoxyhexyl)phenylenediamine (p-TMHPD), by characterising their condensed phase voltammetric properties in aqueous media. The electrochemically driven anion
insertion in p-THPD and p-TMHPD in the presence of ClO4
−, F−, Cl−, Br−, I−, and SO4
2− is shown to be extremely sensitive to structure. The introduction of the methoxy end groups in p-TMHPD causes (1) a considerable shift to more negative electroinsertion potentials, (2) a less stable response which upon
continuous cycling decreases, and (3) considerably lower anion selectivity. For the insertion of sulfate, only p-TMHPD yields an electrochemical response which is shown to be consistent with insertion of the dianion SO4
2−. The electrochemical oxidation of a deposit of m-THPD is accompanied by anion insertion and a chemical reaction step in an EC-type electrochemical process. The product of
the chemical step is electrochemically active and results in a new reversible electroinsertion process. Starting materials
and products of the microdroplet reactions are characterised by Maldi-TOF mass spectrometry and a reaction mechanism based
on condensed phase polymerisation is proposed.
Received: 15 November 1999 / Accepted: 2 December 1999 相似文献
13.
Two long-chain multidentate ligands: 2,9-di-(n-2′,5′,8′-triazanonyl)-1,10-phenanthroline (L1) and 2,9-di-(n-4′,7′,10′-triazaundecyl)-1,10-phenanthroline (L2) were synthesized. The hydrolytic kinetics of p-nitrophenyl phosphate (NPP) catalyzed by complexes of L1 and L2 with La(III) and Gd(III) have been studied in aqueous solution at 298 K, I = 0.10 mol · dm−3 KNO3 at pH 7.5–9.1, respectively. The study shows that the catalytic effect of GdL1 was the best in the four complexes for hydrolysis
of NPP. Its kLnLH−1, k
LnL and pK
a are 0.0127 mol−1 dm3 s−1, 0.000022 mol−1 dm3 s−1 and 8.90, respectively. This paper expounds the result from the structure of the ligands and the properties of the metal
ions, and deduces the catalysis mechanism. 相似文献
14.
Lina Kantiani Marinella Farré Josep Manuel Grases i Freixiedas Damià Barceló 《Analytical and bioanalytical chemistry》2010,398(3):1195-1205
A fully automated method has been developed for analysis of eighteen antibacterial compounds, including penicillins, cephalosporins
and sulfonamides, in animal feed with limits of quantification in the range 0.25–5.79 μg kg−1. The method is based on pressurized liquid extraction of 3 g homogenized feed with water and online clean-up of 500 μL of
the extract with C18HD cartridges. The purified sample was directly analysed by liquid chromatography–electrospray tandem mass spectrometry (SPE–LC–ESI-MS–MS).
Chromatographic separation was achieved within 10 min by use of a C12 Phenomenex Hydro-RP reversed-phase analytical column and a mobile phase gradient (water + 0.1% formic acid–methanol + 0.1%
formic acid). The method was validated, revealing capability for detection of concentrations as low as 0.09 μg kg−1, decision limits (CCα) and detection capabilities (CCβ) in the range 10–174 μg kg−1 and 22–182 μg kg−1, respectively, and inter-day precision ranging from 0.7 to 8.3%. Recovery, with internal standard correction, was in the
range 93–134% for all analytes. The method was then applied to analysis of fifteen feed samples, nine of which contained at
least one antimicrobial at concentrations between 0.006 and 1.526 mg kg−1. The performance data and results from the method were compared with those from a previous method developed by our group,
using offline SPE, by analyzing the same set of samples by both methods. The online SPE approach resulted in slightly improved
sensitivity, with LODs of 0.09–2.12 μg kg−1 compared with 0.12–3.94 μg kg−1 by the offline approach. In general, better recovery was achieved by use of online purification (for 72% of the analytes)
and the correlation between the two methods was good. The main advantages of the new online method are rapid and automated
sample pre-treatment, and reduction of sample manipulation, enabling high-throughput analysis and highly accurate results.
Because of all these characteristics, the proposed method is applicable and could be deemed necessary within the field of
food control and safety. 相似文献
15.
Tomohiro Narukawa Takayoshi Kuroiwa Izumi Narushima Yasujiro Jimbo Toshihiro Suzuki Koichi Chiba 《Analytical and bioanalytical chemistry》2010,397(2):493-499
Arsenate [As(V)] solution reference material, National Metrology Institute of Japan (NMIJ) certified reference material (CRM)
7912-a, for speciation of arsenic species was developed and certified by NMIJ, the National Institute of Advanced Industrial
Science and Technology. High-purity As2O3 reagent powder was dissolved in 0.8 M HNO3 solution and As(III) was oxidized to As(V) with HNO3 to prepare 100 mg kg-1 of As(V) candidate CRM solution. The solution was bottled in 400 bottles (50 mL each). The concentration of As(V) was determined
by four independent analytical techniques—inductively coupled plasma mass spectrometry, inductively coupled plasma optical
emission spectrometry, graphite furnace atomic absorption spectrometry, and liquid chromatography inductively coupled plasma
mass spectrometry—according to As(V) calibration solutions, which were prepared from the arsenic standard of the Japan Calibration
Service system and whose species was guaranteed to be As(V) by NMIJ. The uncertainties of all the measurements and preparation
procedures were evaluated. The certified value of As(V) in the CRM is (99.53 ± 1.67) mg kg-1 (k = 2). 相似文献
16.
Microwave digestion and isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-SFMS) has been applied to the
determination of Pb in rice flour. In order to achieve highly precise determination of low concentrations of Pb, the digestion
blank for Pb was reduced to 0.21 ng g−1 after optimization of the digestion conditions, in which 20 mL analysis solution was obtained after digestion of 0.5 g rice
flour. The observed value of Pb in a non-fat milk powder certified reference material (CRM), NIST SRM 1549, was 16.8 ± 0.8 ng
g−1 (mean ± expanded uncertainty, k = 2; n = 5), which agreed with the certified value of 19 ± 3 ng g−1 and indicated the effectiveness of the method. Analytical results for Pb in three brown rice flour CRMs, NIST SRM 1568a,
NIES CRM 10-a, and NIES CRM 10-b, were 7.32 ± 0.24 ng g−1 (n = 5), 1010 ± 10 ng g−1 (n = 5), and 1250 ± 20 ng g−1 (n = 5), respectively. The concentration of Pb in a candidate white rice flour reference material (RM) sample prepared by the
National Metrology Institute of Japan (NMIJ) was observed to be 4.36 ± 0.28 ng g−1 (n = 10 bottles).
Figure Digestion blank of Pb was carefully reduced to approximately 0.2 ng g-1 which permitted the highly precise determination of Pb at low ng g-1 level in foodstuff samples by ID-SFMS 相似文献
17.
Natalia García-Otero Carmen Teijeiro-Valiño Jacobo Otero-Romaní Elena Peña-Vázquez Antonio Moreda-Piñeiro Pilar Bermejo-Barrera 《Analytical and bioanalytical chemistry》2009,395(4):1107-1115
Nickel(II) and lead(II) ionic imprinted 8-hydroxyquinoline polymers were synthesized by a precipitation polymerization technique
and were used as selective solid phase extraction supports for the determination of nickel and lead in seawater by flow injection
solid phase extraction on-line inductively coupled plasma-optical emission spectrometry. An optimum loading flow rate of 2.25 mL min−1 for 2 min and an elution flow rate of 2.25 mL min−1 for 1 min gave an enrichment factor of 15 for nickel. However, a low dynamic capacity and/or rate for adsorption and desorption
was found for lead ionic imprinted polymer and a flow rate of 3.00 mL min−1 for 4-min loading and a flow rate of 2.25 mL min−1 for 1-min elution gave a enrichment factor of 5. The limit of detection was 0.33 μg L−1 for nickel and 1.88 μg L−1 for lead, with a precision (n = 11) of 8% (2.37 μg Ni L−1) for nickel and 11% (8.38 μg Pb L−1) for lead. Accuracy was also assessed by analyzing SLEW-3 (estuarine water) and TM-24 (lake water) certified reference materials,
and the values determined were in good agreement with the certified concentrations. 相似文献
18.
Berendsen BJ Wegh RS Essers ML Stolker AA Weigel S 《Analytical and bioanalytical chemistry》2012,402(4):1611-1623
A liquid chromatography–tandem mass spectrometry method for the analysis of seven antiviral drugs, zanamivir, ribavirin, oseltamivir,
oseltamivir carboxylate, amantadine, rimantadine and arbidol, in poultry muscle is reported. The antiviral drugs were extracted
from the homogenized poultry muscle sample using methanol. The extract was purified using tandem solid-phase extraction combining
a cation exchange cartridge and a phenylboronic acid cartridge. To prevent excessive matrix effects, the analytes were separated
from the matrix constituents using a column-switch liquid chromatography system combining a reversed-phase and a Hypercarb
analytical column. Detection was carried out using tandem mass spectrometry. The method was fully validated according to 2002/657/EC
[1] and proved to be adequate for quantification and confirmation of zanamivir and ribavirin at 10 μg kg−1, oseltamivir, oseltamivir carboxylate, amantadine and rimantadine at levels below 1.0 μg kg−1 and for qualitative confirmatory analysis of arbidol at levels below 1 μg kg−1. 相似文献
19.
Larivière D Tremblay M Durand-Jézéquel M Tolmachev S 《Analytical and bioanalytical chemistry》2012,403(2):409-418
This article describes a robust methodology using the combination of instrumental design (high matrix interface—HMI), sample
dilution and internal standardization for the quantification of beryllium (Be) in various digested autopsy tissues using inductively
coupled plasma mass spectrometry. The applicability of rhodium as a proper internal standard for Be was demonstrated in three
types of biological matrices (i.e., femur, hair, lung tissues). Using HMI, it was possible to achieve instrumental detection
limits and sensitivity of 0.6 ng L−1 and 157 cps L ng−1, respectively. Resilience to high salt matrices of the HMI setup was also highlighted using bone mimicking solution ([Ca2+] = 26 to 1,400 mg L−1), providing a 14-fold increase in tolerance and a 2.7-fold decrease in method detection limit compared to optimized experimental
conditions obtained without the HMI configuration. Precision of the methodology to detect low levels of Be in autopsy samples
was demonstrated using hair and blood certified reference materials. Be concentration ranging from 0.015 to 255 μg kg−1 in autopsy samples obtained from the U.S. Transuranium and Uranium Registries were measured using the methodology presented. 相似文献
20.
Kinetics of Growth and Enhanced Sophorolipids Production by Candida bombicola Using a Low-Cost Fermentative Medium 总被引:1,自引:0,他引:1
In this study, effect of various parameters on sophorolipid (SL) production by the yeast Candida bombicola was investigated for the enhancing of its production by employing L18 orthogonal array design of experiments. At optimum
conditions of sugarcane molasses 50 g l−1, soybean oil 50 g l−1, inoculum size 5% (v/v), temperature 30 °C, inoculum age 2 days, and agitation 200 rpm, the yeast produced almost equal amounts of the product in
batch shake flasks and in a 3-l fermentor without any pH control (45 and 47 g l−1, respectively). However, the yield increased to 60 g l−1 in the fermentor under controlled pH environment. Time course of SL production, yeast biomass growth, and utilization of
sugarcane molasses and soybean oil at these optimized conditions were fitted to existing kinetic models reported in the literature.
Estimated kinetic parameters from these models suggested that conventional medium containing glucose can very well be replaced
with the present low-cost fermentative medium. 相似文献