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1.
Nawroz Abdul-Razzak Tahir Hoshyar Abdullah Azeez Kadhm Abdullah Muhammad Shewa Anwer Faqe Dlshad Ali Omer 《Natural product research》2019,33(10):1504-1508
The chemical profile of the essential oil of callus and cell suspension cultures derivatives from stem and root of Hypericum triquetrifolium were explored by ITEX/GC-MS. The major constituents for stem derivatives were undecane (78.44%) and 2,4,6-trimethyl-octane (9.74%) for fresh calli, 2,4-dimethyl-benzaldehyde (46.94%), 2,3-dimethyl-undecane (28.39%), 2,4-dimethyl-1-hexene (10.17%), 1,2-oxolinalool (3.64%) and limonene (3.55%) for dry calli and undecane (61.24%), octane, 2,4,6-trimethyl- (16.73%), nonane, 3-methyl-(3.74%), 2,5-diphenyl-benzoquinone (3.70%) and limonene (3.60%) for cell suspension. However, for root derivatives, the dominated components were: undecane (49.94%), eucalyptol (12.07%), limonene (9.98%), toluene (9.03%) and 3-methyl-nonane (4.29%) for fresh calli, 2,4-dimethyl-benzaldehyde (29.80%), 1,1-dimethylethyl-cyclohexane (14.99%), 3-methyl-pentanal (14.99%), undecane (10.04%), beta-terpinyl acetate (8.60%), 1,2-oxolinalool (6.27%) and 2-pentyl-furan (4.09%) for dry calli, undecane (52.38%), 2,4,6-trimethyl-octane (13.81%), 3-methyl-nonane (5.73%), toluene (4.82%) and limonene (4.57%) for cell suspension derivative in root. The attained outcomes indicated that the alkane, aldehyde and monoterpene fractions dominated the chemical composition of essential oils. 相似文献
2.
Formisano C Rigano D Senatore F Bancheva S Bruno M Maggio A Rosselli S 《Natural product communications》2011,6(9):1339-1342
The essential oils of Centaurea gracilenta Velen. (CG) and C. ovina Pall. ex Willd. ssp. besserana (DC.) Dostál (COB) growing wild in Bulgaria, were studied by GC and GC-MS. Forty-five compounds for CG, representing the 90.1% of the oil, and 68 compounds for COB, representing the 91.9% of the oil, were identified. The oils were rich in sesquiterpenoids (33.4% for CG and 27.3% for COB), hydrocarbons (28.3% for CG and 10.7% for COB) and carbonylic compounds (12.7% for CG and 13.1% for COB). Fatty acids were abundant only for COB (31.3%). beta-Eudesmol (12.8%), nonacosane (11.8%) and p-vinyl guiacol (7.5%) were recognized as the main constituents for CG, while hexadecanoic acid (21.4%), spathulenol (7.9%), beta-eudesmol (5.8%) and caryophyllene oxide (5.7%) were the main compounds for COB. 相似文献
3.
The oils of the flowers, stems and leaves of Astrodaucus orientalis L. were separately extracted using hydrodistillation (HD), head-space solid-phase microextraction (HS-SPME) and microwave assisted head-space solid-phase microextraction (MA-HS-SPME). The volatile constituents were analyzed by GC and GC/MS. Temperature and time of extraction, microwave power and exposure time of extraction were optimized. Polydimethylsiloxane (PDMS) fiber was used as the solid phase for SPME methods. The main constituents of the flower, stem and leaf oils isolated by HD, HS-SPME and MA-HS-SPME are as follows, respectively: beta-pinene (20.5%, 13.9% and 30.4%), alpha-thujene (8.7%, 16.2% and 10.9%) and alpha-pinene (7.6%, 14.3% and 10.9%) for the flowers, sabinene (11.8%, 32.3% and 11.8%), alpha-pinene (8.7%, 28.8% and 6.1%) and p-mycrene (2.5%, 12% and 8.5%) for the stem, and alpha-pinene (9.4%, 37.1% and 22.5%), sabinene (13.5%, 26.3% and 23.5%), beta-pinene (6.3%, 9.8% and 10%) and p-mycrene (3.2%, 2.5% and 15.6%) for the leaf. The minimum inhibitory concentrations (MIC) were determined for all essential oils obtained by HD against both Gram-positive (Bacillus subtilis) and Gram-negative (Escherichia coli) bacteria using the agar dilution method. These oils showed the good activities against the both bacteria (0.5 - 1.5 mg/mL). 相似文献
4.
The method of MacMahon and Lohne for analysis of nitrofuran metabolites in shrimp was optimized to streamline the extraction processes and the LC analysis. This revised method includes 16 h of mild acid hydrolysis/derivatization followed by ethyl acetate extraction and analysis by LC/MS/MS in the atmospheric pressure chemical ionization mode. This revised method was validated in shrimp for concentrations of 0.25 to 2.0 ng/g. The LOQ was 0.25 ng/g for all metabolites. The LOD was 0.052 nglg for 1-aminohydantoin (AHD), 0.206 ng/g for 3-amino-2-oxazolidinone (AOZ), 0.108 ng/g for semicarbazide (SC), and 0.062 ng/g for 3-amino-5-morpholinomethyl-2-oxazolidinone (AMOZ). The spike recoveries with RSD into negative matrix at 1 ng/g were 100.2% (3.2%) for AHD, 102.5% (1.0%) for AOZ, 103.7% (2.3%) for SC, and 104.0% (3.3%) for AMOZ. The spike recoveries at 1 ng/g into unknown samples (n=108) containing varied levels of nitrofuran metabolites were 112.6% (25.7%) for AHD, 108.1% (12.1%) for AOZ, 103.0% (12.0%) for SC, and 100.3% (6.9%) for AMOZ. Interday precision with samples containing incurred AOZ concentrations of 0.92 to 17.8 ppb performed over a year was 10.4% RSD. The method is accurate and precise for determining nitrofuran concentrations in the edible tissue of shrimp. 相似文献
5.
Richardson RK 《Journal of AOAC International》2001,84(5):1522-1533
Gravimetric fat data were obtained for a wide range of dairy products with fat contents ranging from 0.5 to 83% using pressurized solvent extraction at elevated temperatures and pressure (80-120 degrees C; 10.3 MPa). Extraction performance was sensitive to solvent composition, temperature, and sample matrix. By optimizing solvent mixtures, sample-solvent contact times of 8-10 min were sufficient for high recoveries from all products tested. The most successful solvents with regard to speed of extraction, selectivity, and recovery (average recovery, %) were various mixtures of hexane (or petroleum ether)-dichloromethane-methanol for dried cream (99.8%), dried whole milk (99.6%), dried buttermilk (98.2%), dried skim milk (97.0%), dried whey protein concentrate (97.5%), casein (95.0%), and caseinate (102.1%); petroleum ether-acetone-ethanol or petroleum ether-acetone-isopropanol for cheddar-type cheese (99.4%); petroleum ether-acetone for butter (99.9%); petroleum ether-acetone-isopropanol for cream (100.3%); and petroleum ether-isopropanol for liquid milks (99.0%). Relative standard deviations for repeatability were obtained for dried whole milk (0.2%), dried whey protein concentrate (0.7%), cheese (0.3%), butter (0.1%), and ultraheat treated (UHT) milk (0.7%). Solvent removal and drying of extracts with a heated block evaporator saved time compared with conventional drying ovens. Estimated savings in labor (50-75%) and solvents (80%) were substantial compared with the manual Mojonnier methods. 相似文献
6.
The effects of 150 kilogray (kGy) of γ irradiation on cell-wall constituents of cottonwood (CW), lentils straw (LS), apple pruning products (AP) and olive cake (OC) were investigated. Samples were irradiated by γ irradiation at a dose level of 150 kGy under identical conditions of temperature and humidity and analyzed for crude fibre (CF), neutral-detergent fibre (NDF), acid detergent fibre (ADF) and acid-detergent lignin (ADL). The results indicate that γ irradiation decreased CF contents by about 29% for CW, LS and AP and by 17% for OC. NDF values were also decreased by about 4% for CW and OC, and by about 12% for LS and AP. γ Irradiation treatment also decreased ADF values only for CW by 8%. ADL contents decreased by 8% for CW and 5% for OC with no effects for LS and AP. The percentage of cellulose (CL): CF ratio increased by 30, 34, 38 and 20% for CW, LS, AP and OC, respectively. Also, the percentage of hemicellulose (HCL): CF increased by 57% for CW and 16% for OC and decreased by 7% for LS and AP. The percentage of HCL: ADL increased by 22% for CW but decreased by 33% for LS and AP with no changes for OC. There were no changes in CL: ADL ratio for all residues. 相似文献
7.
CHEN Feng DONG Dan FU Yan ZHENG Yong-hui LIU Shi CHANG Ming-xin JING Xia-bin 《高等学校化学研究》2012,28(4):656-661
Two kinds of paclitaxel(PTX) conjugate micelles, of which one contained 25%(mass fraction) PTX [M(PTX)] and the other contained 22.5%(mass fraction) of PTX and 1.4%(mass fraction) of folate(FA)[FA-M(PTX)], were prepared for cell apoptosis and anti-tumor activity evaluation on U14 cervical cancer mouse models in comparison with 0.9%(mass fraction) saline(control) and equivalent Taxol. Seven days after tail intravenous injection of the drugs, the mice were sacrificed to measure the tumor masses. The average tumor masses were 4.26, 2.89, 2.63, and 2.17 g for the control, Taxol, M(PTX) and FA-M(PTX) groups, respectively. The inhibition rates of tumor growth calculated for the three drug groups were 32%, 38% and 49%, respectively. Flow cytometry(FC) analysis and termi- nal deoxynucleotidyl transferase(TdT)-mediated deoxyuridine triphosphate(dUTP) nick end labeling(TUNEL) assay were conducted on the cancer tissues. The cell apoptosis rates based on the FC data and the TUNEL data were 20%, 31%, 37%, 42%, and 10%, 22%, 26%, 34%, respectively, both showing statistically significant differences(P<0.05) between three drug groups and the control group, and between the FA-M(PTX) group and the other two drug groups. In conclusion, the composite FA-M(PTX) micelles can be used for U14 cervical cancer treatment. 相似文献
8.
Simultaneous determination of major,minor and trace elements in biocarbonates by inductively coupled plasma mass spectrometry 总被引:2,自引:0,他引:2
A method was developed for simultaneous determination of major (Ca), minor (Mg and Sr) and trace (Ba and U) elements in biocarbonates by inductively coupled plasma mass spectrometry (ICP-MS). The method precision (RSD%) is 0.73% for Ca, 0.77% for Mg, 0.59% for Sr, 2.02% for Ba, 1.13% for U, 0.67% for Mg/Ca, 0.27% for Sr/Ca, 2.06% for Ba/Ca and 1.23% for U/Ca. The ratio precision suggests that ICP-MS is satisfactory for obtaining multi-ratio data from biocarbonates. This technique was applied to 67 continuous coral samples. 相似文献
9.
A reversed-phase liquid chromatographic method was developed and validated for the determination of the content of free acetic acid, free succinic acid, acetyl substituents, and succinoyl substituents in hydroxypropyl methylcellulose acetate succinate (HPMCAS; Chemical Abstracts Service Registry No. 71138-97-1) polymer. This single new method gave accurate and precise measurement of both acetyl and succinoyl substituents, which had previously required 3 Japanese Pharmaceutical Excipients (JPE) methods to accomplish. Consequently, analysis time and turnaround time are decreased significantly. Furthermore, this method can also separate and determine the free acetic and succinic acids in HPMCAS polymer, a task that the corresponding JPE method cannot achieve. The values for accuracy (average recovery from 12 standard samples) were 99.9% for acetic acid and 99.8% for succinic acid. The values for injection precision (relative standard deviation [RSD]) were 0.11% for acetic acid and 0.28% for succinic acid. The values for intermediate precision (RSD) were 1.25% for determination of the acetyl content at the 8.78% (w/w) level and 1.33% for determination of the succinoyl content at the 10.9% (w/w) level. The values for intermediate precision (RSD) were 5.98% for determination of free acetic acid at the 0.12% (w/w) level and 5.13% for determination of free succinic acid at the 0.029% (w/w) level. The method was proven to be robust with respect to variation in the pH of the mobile phase, the concentration of potassium dihydrogen phosphate, and the flow rate. The method is well suited for quality control in today's fast-paced pharmaceutical laboratories. 相似文献
10.
Yingjun Kong Xiunan Li Gaoying Bai Guanghui Ma Zhiguo Su 《Journal of chromatography. A》2010,1217(44):6898-6904
An automatic system for multidimensional integrated protein chromatography was designed for simultaneous separation of multiple proteins from complex mixtures, such as human plasma and tissue lysates. This computer-controlled system integrates several chromatographic columns that work independently or cooperatively with one another to achieve efficient high throughputs. The pipelines can be automatically switched either to another column or to a collection container for each UV-detected elution fraction. Environmental contamination is avoided due to the closed fluid paths and elimination of manual column change. This novel system was successfully used for simultaneous preparation of five proteins from the precipitate of human plasma fraction IV (fraction IV). The system involved gel filtration, ion exchange, hydrophobic interaction, and heparin affinity chromatography. Human serum albumin (HSA), transferrin (Tf), antithrombin-III (AT-III), alpha 1-antitrypsin (α1-AT), and haptoglobin (Hp) were purified within 3 h. The following recovery and purity were achieved: 95% (RSD, 2.8%) and 95% for HSA, 80% (RSD, 2.0%) and 99% for Tf, 70% (RSD, 2.1%) and 99% for AT-III, 65% (RSD, 2.0%) and 94% for α1-AT, and 50% (RSD, 1.0%) and 90% for Hp. The results demonstrate that this novel multidimensional integrated chromatography system is capable of simultaneously separating multiple protein products from the same raw material with high yield and purity and it has the potential for a wide range of multi-step chromatography separation processes. 相似文献
11.
《Analytical letters》2012,45(9):1933-1941
Abstract Ranitidine hydrochloride in tablets (T) and injections (I) was determined by ultraviolet spectrophotometry (UVS) at 313 nm and visible spectrophotometry (VISS) at 615 nm, after reaction with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) and ferric chloride. For UVS, Beer's law was obeyed in the range 5.0 – 18.0 μg/mL. The coefficients of variation (CV) for the samples T were 0.36% and 0.71% and for the samples I were 0.51% and 0.24%. The recovery average (RA) was 99.88%. For UVS, Beer's law was observed in the range 1.44 – 5.76 μg/mL. The CV for T were 0.72% and 0.59%, and for I were 0.53% and 0.61%. The RA was 99.39%. The precision and accuracy of the two methods were compared. 相似文献
12.
Comparison of aqua regia and HNO3-H2O2 procedures for extraction of Tl and some other elements from soils 总被引:1,自引:0,他引:1
Pavlícková J Zbíral J Cizmárová E Kubán V 《Analytical and bioanalytical chemistry》2003,376(1):118-125
The relationship between aqua regia (ISO 11466) and HNO(3)-H(2)O(2) (ISO/CD 20279) extraction procedures for atomic emission spectrometric (ICP/OES and ICP/MS) determinations of Tl, P, Mn, Fe, Mg, Ca, Sr, Al, K, As, Bi, Zn, Pb, Co, Cd, Ni, V, Be, Cu and Cr was investigated. Soil samples (155) representing areas with different contents of the elements were selected for the comparison. Tl was the element of the highest interest and therefore the sampling sites were chosen to achieve as wide range of Tl contents as possible. Both extraction procedures are comparable in results (differences lower than 10% for the most of the elements) for all the tested elements. Statistically non-significant differences between the two extraction procedures were found for P, Zn, V and K (the slope was very close to 1 and the intercept included zero). Statistically significant values of intercepts were found for Fe, Al, Ca, Cd, Sr and Ni. Significantly higher results for aqua regia were found for Cu (12%), Pb (17%), Mn (11%) and lower results by aqua regia were found for Mg (4%), As (13%), Co (20%), Be (11%), Cr (4%) and Bi (6%). The results for Tl, the element of the highest interest, after HNO(3)-H(2)O(2) extraction procedure, were approximately 6% higher than the results after aqua regia extraction. Content of Tl in the soil samples was from 0.08 to 2.8 mg kg(-1). A highly significant linear relationship was found (R(2)=0.97). 相似文献
13.
A HPLC method with diode-array detection, at 265 nm, was developed and validated for the determination of ten sulfonamides (SAs): sulfadiazine (SDZ), sulfathiazine (STZ), sulfamethoxine (SMTH), sulfamethizole (SMZ), sulfamethoxypyridazine (SMPZ), sulfamonomethoxine (SMMX), sulfamethoxazole (SMXZ), sulfisoxazole (SIX), sulfadimethoxine (SDMX), and sulfaquinoxaline (SQX) in milk. A mixture of ethyl acetate, n-hexane, and isopropanol was used for the extraction of target analytes from milk. The mobile phase, a mixture of 0.1% v/v formic acid, CH(3) CN, and CH(3) OH was delivered to the analytical column under a gradient program. The procedure was validated according to the European Union regulation 2002/657/EC in terms of selectivity, stability, decision limit, detection capability, accuracy, and precision. Mean recoveries of sulfonamides from milk samples spiked at three concentration levels (0.5×MRL, 1×MRL, and 1.5×MRL) (MRL, maximum residue level) were 93.9-115.9% for SDZ, 97.8-102.9% for STZ, 94.6-107.0% for SMTH, 98.3-111.5% for SMZ, 95.3-108.4% for SMPZ, 97.9-106.0% for SMMX, 97.6-111.3% for SMXZ, 94.3-104.6% for SIX, 96.4-109.1% for SDMX, and 98.2-111.2% for SQX. All RSD values were lower than 8.8%. The decision limits CCa calculated by spiking 20 blank milk samples at MRL (100 μg/kg) ranged from 101.61 to 106.84 μg/kg, whereas the detection capability CCb ranged from 105.64 to 119.01 μg/kg. 相似文献
14.
Chatterjee A 《Talanta》2000,51(2):303-314
A microwave-assisted digestion procedure was developed in presence of concentrated nitric acid (2.0 ml) and 30% hydrogen peroxide (0.20 ml) using a closed pressurized microwave digestion system for the determination of total anionic and total cationic arsenic compounds reside in oyster tissue. At 450 W for 15 min digestion, 74% of anionic arsenic, and 31% of cationic arsenic (105% total arsenic) were retrieved. At 300 W microwave power, 68% of anionic and 30.5% of cationic arsenic (98.5% total arsenic), and 100 W, 63% of anionic and 31% of cationic arsenic (94% total arsenic) were extracted out. The methanol water mixture (9:1) was cull out, exclusively 31.6% of anionic and 29% of cationic arsenic compounds (60.6% total). The dimethylarsinoylriboside (phosphate-arsenosugar) was the predominant arsenic species, along with arsenobetaine (AB), dimethylarsinic acid (DMA), inorganic arsenic, methylarsonic acid (MA), arsenocholine (AC), trimethylarsineoxide (TMAO) and tetramethylarsonium ion (TMI). Some other arsenic compounds, those were not matched with the retention time of the available standards, were also detected. Arsenosugar was fragile and adequately transmuted to DMA (100%), AB and AC to TMAO (100%) when 450 W microwave power was applied for 15 min. The separation and quantification of arsenic compounds in the microwave digests and extracts, were carried out in anion (PRP-X100) and cation (LC-SCX) exchange columns using ICP-MS as arsenic specific detector. The procedure was also validated by determining the total cationic and total anionic arsenic compounds present in DORM 1. 相似文献
15.
Mezyk SP Neubauer TJ Cooper WJ Peller JR 《The journal of physical chemistry. A》2007,111(37):9019-9024
Absolute rate constants and degradation efficiencies for hydroxyl radical and hydrated electron reactions with four different sulfa drugs in water have been evaluated using a combination of electron pulse radiolysis/absorption spectroscopy and steady-state radiolysis/high-performance liquid chromatography measurements. For sulfamethazine, sulfamethizole, sulfamethoxazole, and sulfamerazine, absolute rate constants for hydroxyl radical oxidation were determined as (8.3 +/- 0.8) x 10(9), (7.9 +/- 0.4) x 10(9), (8.5 +/- 0.3) x 10(9), and (7.8 +/- 0.3) x 10(9) M(-1) s(-1), respectively, with corresponding degradation efficiencies of 36% +/- 6%, 46% +/- 8%, 53% +/- 8%, and 35% +/- 5%. The reduction of these four compounds by their reaction with the hydrated electron occurred with rate constants of (2.4 +/- 0.1) x 10(10), (2.0 +/- 0.1) x 10(10), (1.0 +/- 0.03) x 10(10), and (2.0 +/- 0.1) x 10(10) M(-1) s(-1), respectively, with efficiencies of 0.5% +/- 4%, 61% +/- 9%, 71% +/- 10%, and 19% +/- 5%. We propose that hydroxyl radical adds predominantly to the sulfanilic acid ring of the different sulfa drugs based on similar hydroxyl radical rate constants and transient absorption spectra. In contrast, the variation in the rate constants for hydrated electrons with the sulfa drugs suggests the reaction occurs at different reaction sites, likely the different heterocyclic rings. The results of this study provide fundamental mechanistic parameters, hydroxyl radical and hydrated electron rate constants, and degradation efficiencies that are critical for the evaluation and implementation of advanced oxidation processes (AOPs). 相似文献
16.
Kowalczuk D 《Journal of AOAC International》2005,88(5):1525-1529
A high-performance thin-layer chromatography (TLC) method coupled with densitometric analysis has been developed for simultaneous measurement of trandolapril (TRA) and verapamil (VER) in 2-component mixtures and in their combination capsules. The active substances were extracted from capsules with methanol (mean recovery: 103.4% for TRA, 97.13% for VER) and chromatographed on TLC plates coated with silica gel 60 F254 in horizontal chambers with ethyl acetatc-ethanol-acetic acid (8 + 2 + 0.5, v/v) mobile phase. Chromatographic separation of these components was followed by ultraviolet densitometric quantification at 215 nm. The calibration graphs were constructed over the concentration range from 0.5 to 1.5 microg/microL (corresponding to 5.0-15.0 microg/spot) for both drugs with good correlation (r > or = 0.990). Detection and quantitation limits were found to be 1.25 and 3.75 microg/spot for TRA and 0.15 and 0.45 microg/spot for VER, respectively. The proposed method was used for determination of both drugs in TRA-VER capsules with satisfactory precision [0.97% < relative standard deviation (RSD) < 4.50% for TRA, 0.49% < RSD < 3.10% for VER] and accuracy [2.16% < relative error (RE) < 4.90% for TRA, 1.73% < RE < 5.68% for VER]. 相似文献
17.
4,4'-Bis(dihexylaminocarbonyl)-2,2'-bipyridine (BDC-Bipy) was synthesized and studied systematically as a chelating reagent for metal ions extraction in supercritical CO(2). The compound showed high extraction efficiency for Co(2+) (100%), Cu(2+) (100%), Cd(2+) (98.2%), and Zn(2+) (100%) ions and good extraction efficiency for Sr(2+) (79.4%) and Pb(2+) (89.8%) when the extraction was performed in supercritical CO(2) at 313 K and 25 MPa with the system of BDC-Bipy, deionized water and perfluoro-1-octanesulfonic acid tetraethylammonium salt. The recoveries of mixed metal ions were also measured; unfortunately, the system of extraction has no selectivity for the metal ions. 相似文献
18.
19.
Chitescu CL Oosterink E de Jong J Linda Stolker AA 《Analytical and bioanalytical chemistry》2012,403(10):2997-3011
The use of pharmaceuticals in livestock production is a potential source of surface water, groundwater and soil contamination. Possible impacts of antibiotics on the environment include toxicity and the emergence of antibiotic resistance. Monitoring programs are required to record the presence of these substances in the environment. A rapid, versatile and selective multi-method was developed and validated for screening 43 pharmaceutical and fungicides compounds, in surface and groundwater, in one single full-scan MS method, using benchtop U-HPLC-Exactive Orbitrap MS at 50,000 (FWHM) resolution. Detection was based on calculated exact masses and on retention time. Sample volume, pH conditions and solid-phase extraction (SPE) sample clean-up conditions were optimized. In the final method, 74 % of the compounds had recoveries higher than 80 %, 15 % of the compounds had recoveries between 60 % and 80 %, and 7 % of the compounds had recoveries between 40 % and 50 %. One of the compounds (itraconazole) had a recovery lower than 10 % and nystatin was not detected. The level of detection was 10 ng L(-1) for 61 % of the compounds, 50 ng L(-1) for 32 % and 100 ng L(-1) for 5%. In-house validation, based on EU guidelines, proves that the detection capability CCβ is lower than 10 ng L(-1) (for β error 5 %) for 37 % of the compounds, lower than 50 ng L(-1) for 35 % of the compounds and lower than 100 ng L(-1) for 14 % of compounds. This study demonstrates that the ultra-high resolution and reliable mass accuracy of Exactive Orbitrap MS permits the detection of pharmaceutical residues in a concentration range of 10-100 ng L(-1), applying a post target screening approach, in the multi-method conditions. 相似文献
20.
Dai FR Wu WJ Wang QW Tian H Wong WY 《Dalton transactions (Cambridge, England : 2003)》2011,40(10):2314-2323
Four new heteroleptic ruthenium sensitizers [Ru(4,4'-carboxylic acid-2,2'-bipyridine)(L)(NCS)(2)] (L = 5,5'-bis(4-octylthiophen-2-yl)-2,2'-bipyridine (1), 5,5'-bis(N,N-diphenyl-4-aminophenyl)-2,2'-bipyridine (2), 5,5'-bis(5-(N,N-diphenyl-4-aminophenyl)-thiophen-2-yl)-2,2'-bipyridine (3) and 5,5'-bis(4-octyl-5-(N,N-diphenyl-4-aminophenyl)-thiophen-2-yl)-2,2'-bipyridine (4)) were synthesized, characterized by physicochemical and computational methods, and utilized as photosensitizers in nanocrystalline dye-sensitized solar cells (DSSCs). The λ(max) of the metal-to-ligand charge transfer (MLCT) absorption of these four ruthenium dyes (527 nm for 1, 535 nm for 2, 585 nm for 3 and 553 nm for 4) can be tuned by various structural modifications of the ancillary ligand and it was shown that increasing the conjugation length of such ligand reduces the energy as well as the molar absorption coefficient of the MLCT band. The maximum incident photon to current conversion efficiency (IPCE) of 41.4% at 550 nm, 38.6% at 480 nm, 39.4% at 470 nm and 31.1% at 480 nm for 1-, 2-, 3- and 4-sensitized solar cells were obtained. Respectable power conversion efficiencies of 3.00%, 2.51%, 2.00% and 2.03% were realized, respectively, when the sensitizers 1, 2, 3 and 4 were used in DSSCs under the standard air mass (AM) 1.5 sunlight illumination (versus 5.9% for standard N719). 相似文献