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921.
Gemechu Zeleke Siegrid De Baere Sultan Suleman Mathias Devreese 《Molecules (Basel, Switzerland)》2022,27(3)
A fast, accurate and reliable ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) method was developed for simultaneous quantification of ivermectin (IVER), doramectin (DORA), and moxidectin (MOXI) in bovine plasma. A priority for sample preparation was the eradication of possible infectious diseases to avoid travel restrictions. The sample preparation was based on protein precipitation using 1% formic acid in acetonitrile, followed by Ostro® 96-well plate pass-through sample clean-up. The simple and straightforward procedure, along with the short analysis time, makes the current method unique and suitable for a large set of sample analyses per day for PK studies. Chromatographic separation was performed using an Acquity UPLC HSS-T3 column, with 0.01% acetic acid in water and methanol, on an Acquity H-Class ultra-high performance liquid chromatograph (UHPLC) system. The MS/MS instrument was a Xevo TQ-S® mass spectrometer, operating in the positive electrospray ionization mode and two multiple reaction monitoring (MRM) transitions were monitored per component. The MRM transitions of m/z 897.50 > 753.4 for IVER, m/z 921.70 > 777.40 for DORA and m/z 640.40 > 123.10 for MOXI were used for quantification. The method validation was performed using matrix-matched calibration curves in a concentration range of 1 to 500 ng/mL. Calibration curves fitted a quadratic regression model with 1/x2 weighting (r ≥ 0.998 and GoF ≤ 4.85%). Limits of quantification (LOQ) values of 1 ng/mL were obtained for all the analytes, while the limits of detection (LOD) were 0.02 ng/mL for IVER, 0.03 ng/mL for DORA, and 0.58 ng/mL for MOXI. The results of within-day (RSD < 6.50%) and between-day (RSD < 8.10%) precision and accuracies fell within acceptance ranges. No carry-over and no peak were detected in the UHPLC-MS/MS chromatogram of blank samples showing good specificity of the method. The applicability of the developed method was proved by an analysis of the field PK samples. 相似文献
922.
Bing-Yu Li Lauren Voets Ruben Van Lommel Fien Hoppenbrouwers Mercedes Alonso Steven H. L. Verhelst Wim M. De Borggraeve Joachim Demaerel 《Chemical science》2022,13(8):2270
Sulfur(vi) Fluoride Exchange (SuFEx) chemistry has emerged as a next-generation click reaction, designed to assemble functional molecules quickly and modularly. Here, we report the ex situ generation of trifluoromethanesulfonyl fluoride (CF3SO2F) gas in a two chamber system, and its use as a new SuFEx handle to efficiently synthesize triflates and triflamides. This broadly tolerated protocol lends itself to peptide modification or to telescoping into coupling reactions. Moreover, redesigning the SVI–F connector with a S O → S NR replacement furnished the analogous triflimidoyl fluorides as SuFEx electrophiles, which were engaged in the synthesis of rarely reported triflimidate esters. Notably, experiments showed H2O to be the key towards achieving chemoselective trifluoromethanesulfonation of phenols vs. amine groups, a phenomenon best explained—using ab initio metadynamics simulations—by a hydrogen bonded termolecular transition state for the CF3SO2F triflylation of amines.Triflyl fluoride gas (CF3SO2F) and its aza analogues are reported as new SuFEx activators. These SVI–F reagents react efficiently with a variety of nucleophiles, yet the presence of water grants complete chemoselectivity to phenols. 相似文献
923.
R. De Souza D. Neibecker I. Tkatchenko G. Boiteux A. Revillon 《Macromolecular Symposia》1989,24(1):137-143
Monometallic complexes of Nickel have been successfully, tested in reaction with olefinic and acetylenic compounds. This paper is devoted to one of the resulting products, a polyphenylacetylene which presents interesting properties. It is readily obtained avoiding the step of a polymer precursor; it is soluble in several solvents, stable in air up to 200° C and may possess a rather high conductivity, depending on polymerization conditions. This is a noticeable difference versus previously reported polyphenylacetylenes which were insulating materials. 相似文献
924.
Rapid and high-performance analysis of thyreostatic drug residues in urine using gas chromatography-mass spectrometry 总被引:1,自引:0,他引:1
Peter Batjoens Hubert F. De Brabander Katia De Wasch 《Journal of chromatography. A》1996,750(1-2):127-132
A more sensitive method was developed using the hyphenated technique of gas chromatography-mass spectrometry (GC-MS) supplementary to the official high-performance thin-layer chromatography (HPTLC) method. Even combined with less efficient extraction and clean-up methods, GC-MS is able to lower the detection limit to less than 50 ppb. The powerful technique of GC-MS-MS is tried out to reduce the detection limit even more, in combination with simplified extraction methods. This time-saving approach combined with the increase in sensitivity is of great importance for a routine technique. 相似文献
925.
The determination of biogenic amines in alcoholic beverages is important to assess the potential risks associated with the consumption of high concentrations of these compounds. In addition, product storage conditions and the length of storage can cause the formation of biogenic amines that reduce product quality. We report a new method using cation-exchange chromatography with either suppressed conductivity, integrated pulsed amperometry, UV, or a combination of these detection techniques to determine biogenic amines in alcoholic beverages. The main objective was to provide a direct comparison between IPAD and suppressed conductivity detection for determining biogenic amines in alcoholic beverages. Suppressed conductivity is the simplest detection approach for determining putrescine, cadaverine, histamine, agmatine, phenylethylamine, spermidine, and spermine with good sensitivity (0.004-0.08 mg/l) and was used to evaluate the influence of storage time and conditions on the evolution of biogenic amines in alcoholic beverages. Integrated pulsed amperometric detection (IPAD) detects more biogenic amines than suppressed conductivity detection, enabling the detection of dopamine, tyramine, and serotonin. Tyramine was simultaneously determined by UV detection and IPAD to provide confirmation and ensure the accuracy of the analytical results. The linearity of biogenic amine responses was within 0.1-20 mg/l and peak area precisions were 0.24-4.97% for IPAD, suppressed conductivity-IPAD, and UV detection. The sensitivity for the 10 biogenic amines using the 3 detection techniques varied considerably from 0.004-1.1 mg/l and recoveries were within 85-122%. 相似文献
926.
George R. De Mar 《Journal of Molecular Structure》1987,160(3-4):327-335
Ab initio optimizations of the complete acrolein molecular geometry accomplished using analytical gradient methods at the 6-31G* SCF level at ten points during rotation from the planar trans- to the planar cis-form (rotation about the single C---C bond) are used to calculate the values of the Pitzer function F(φ), the coefficients of its Fourier expansion, and the coefficients in the potential energy expansion. The theoretical potential expansion coefficients are then adjusted using the experimental torsional frequencies and their overtones for the trans- and cis-forms of CH2=CH---CH=O and CH2=CH---CD=O. For the cis-conformer two different sets of experimental frequencies are employed. The dependence of the slope of the acrolein potential energy curve on the experimental frequency set used for the cis-rotamer is discussed. 相似文献
927.
Amyloglucosidase from Novo (Copenhagen, Denmark) was immobilized in controlled pore silica particles with the silane-glutaraldehyde
covalent method. Thermal stability of the free and immobilized enzyme (IE) was determined with 30% (w/v) α-amylase liquefied
cassava starch, pH 4.5, temperatures from 35 to 75°C. Free amyloglucosidase maintained its activity practically constant for
240 min and temperatures up to 50°C. The IE has shown higher stability retaining its activity for the same period up to 60°C.
Half-life for free enzyme was 20.6, 6.44, 2.07, 0.69, and 0.24 h for 55, 60, 65, 70, and 75°C, respectively, whereas the IE
at the same temperatures had half-lives of 116.4, 30.88, 8.52, 2.44, and 0.73 h. The energy of thermal deactivation was thus
50.6 and 57.6 kcal/mol, respectively for the free and IE, confirming stabilization by immobilization. 相似文献
928.
J. Mullens A. Vos A. De Backer D. Franco J. Yperman L. C. Van Poucke 《Journal of Thermal Analysis and Calorimetry》1993,40(1):303-311
The 124 superconductor YBa2Cu4O8 was prepared from the oxalate precursor Y2(C2O4)3. ·4BaC2O4·8CuC2O4·xH2O at one atmosphere oxygen pressure. In O2 the precursor decomposes in one step at 300°C and more gradually (300°–600°C) in Ar. The stability of the superconductor is strongly dependent on the gas atmosphere: in O2 and in air there is no significant weight change as long as the temperature does not exceed 800°C, whereas in a 1% O2-99%N2 mixture decomposition starts at about 670°C with the formation of CuO and YBa2Cu3Ox withx<7. The reduction of YBa2Cu4O8 in a 5% H2-95% Ar mixture takes place in at least four major steps with formation of products such as Y2O3, BaO, Cu2O, Cu, BaY2O4 and Ba4Y2O7. 相似文献
929.
采用体积排斥色谱法/ 示差折光指数/ 直角激光光散射/ 示差粘度三检测联用技术表征了氘化聚苯乙烯、聚苯乙烯和氘化聚苯乙烯- 聚异戊二烯。结果表明,在θ条件下,虽然氘化聚苯乙烯的化学依赖性常数υT,DPS比聚苯乙烯的化学依赖性常数υT,PS大,但25 ℃时在四氢呋喃中,氘化聚苯乙烯的分子尺寸仍小于聚苯乙烯的分子尺寸。由于嵌段共聚物的淋洗体积随组成变化,所以用传统的SEC/RI得不到准确的分子量。经比较膜渗透、小角激光光散射和基质辅助激光脱吸与离子化时间飞行质谱等的实验结果,证明体积排斥色谱法/ 示差折光指数/ 直角激光光散射/ 示差粘度三检测技术能准确地得到氘化二嵌段共聚物的分子量以及其它重要信息。 相似文献
930.
Jian‐Gong Yang Kai Li Jian Wang Shanshan Sun Weijie Chi Chao Wang Xiaoyong Chang Chao Zou Wai‐Pong To Ming‐De Li Xiaogang Liu Wei Lu Hong‐Xing Zhang Chi‐Ming Che Yong Chen 《Angewandte Chemie (International ed. in English)》2020,59(17):6915-6922
Materials exhibiting excitation wavelength‐dependent photoluminescence (Ex‐De PL) in the visible region have potential applications in bioimaging, optoelectronics and anti‐counterfeiting. Two multifunctional, chiral [Au(NHC)2][Au(CN)2] (NHC=(4R,5R)/(4S,5S)‐1,3‐dimethyl‐4,5‐diphenyl‐4,5‐dihydro‐imidazolin‐2‐ylidene) complex double salts display Ex‐De circularly polarized luminescence (CPL) in doped polymer films and in ground powder. Emission maxima can be dynamically tuned from 440 to 530 nm by changing the excitation wavelength. The continuously tunable photoluminescence is proposed to originate from multiple emissive excited states as a result of the existence of varied AuI???AuI distances in ground state. The steric properties of the NHC ligand are crucial to the tuning of AuI???AuI distances. An anti‐counterfeiting application using these two salts is demonstrated. 相似文献