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1.
Tomáš Hložek Martin Štícha Miroslava Bursová Ivan Jelínek Petr Tůma Radomír Čabala 《Electrophoresis》2020,41(18-19):1564-1567
Riociguat is novel antihypertensive drug for treatment of pulmonary hypertension. As such, it is still being tested in many clinical and pharmacokinetic trials. Existing methods that determine serum riociguat and desmethylriociguat (DMR) are based solely on liquid chromatography with mass spectrometry. Therefore, we present a novel capillary electrophoresis with mass spectrometry method (CE-MS) for their determination in human serum as alternative method for ongoing trials. Complete resolution of both analytes was achieved by means of pH optimization of ammonium formate background electrolytes that are fully compatible with ESI/MS detection. Simple liquid-liquid extraction was used as sample pretreatment. The calibration dependence of the method was linear (in the range of 10–1000 ng/mL), with adequate accuracy (90.1–114.9%) and precision (13.4%). LOD and LOQ were arbitrarily set at 10 ng/mL for both analytes. Clinical applicability was validated using serum samples from patients treated with riociguat in pharmacokinetic study and the results corresponded with reference HPLC-MS/MS values. Capillary electrophoresis proved to be sensitive and selective tool for the analysis of riociguat and DMR. 相似文献
2.
The Efficient Determination Criterion (EDC) generalizes the AIC and BIC criteria and provides a class of consistent estimators
for the order of a Markov chain with finite state space. In this note, we derive rates of convergence for the EDC estimates.
*Partially supported by CNPq, CAPES/PROCAD, FAPDF/PRONEX, FINATEC and FUNPE/UnB.
**Partially supported by CAPES. 相似文献
3.
4.
在氨性介质中(pH=9.0),钴(Ⅱ)-丁二酮单肟烟酰腙(DMNH)-亚硝酸盐体系可产生灵敏度很高的催化波。从体系的伏安行为可知,吸附于汞电极上的是混配的配盐NH_4[Co(Ⅱ)(DMNH)·(NO_2)_2],在-1.0 V(相对SCE)处,Co(Ⅱ)被还原至Co(0),DMNH被还原成自由基,由于NO_2~-的存在,自由基可参与再生反应而形成催化波。羟氨的存在可使产生催化波的最佳pH值移至8.2.用此体系进行了生物样品中钴的测定,其检出限为1×10~(-10)mol/L。 相似文献
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6.
氢化物原子荧光法(HG-AFS)测定鸡蛋中的硒 总被引:4,自引:0,他引:4
本文建立了一种HG-AFS法测定食疗蛋中硒的方法,该方法简单,快速,同时也提高了分析的灵敏度。方法的检出限为0.3μg/L,食疗蛋中硒的样品测定的相对标准偏差<10%,回收率在90%以上。 相似文献
7.
《Electroanalysis》2006,18(22):2218-2224
This article deals with the development of a method for the determination of osmium at a carbon paste electrode (CPE) modified with cationic surfactants of the quaternary ammonium salt type; namely, cetyltrimethylammonium bromide (CTAB) and 1‐(ethoxycarbonyl)‐pentadecyltrimethyl‐ammonium bromide (Septonex); both being added in situ and serving for preconcentration of osmium via its hexachloroosmate(IV) anion. The proper electrochemical detection was performed by cathodic scanning in the differential pulse voltammetric mode. Optimization studies concerning important experimental parameters also included a specially performed potentiometric titration, helping to define the actual stoichiometry for the ion‐pairing process, the main principle and driving force of the accumulation step. In a chloride/acetate buffer based supporting medium and with Septonex as the modifier of choice, the reduction signal for osmium was found to be proportional to the Os(IV) concentration in a range from 5×10?9 to 5×10?7 mol L?1 with a limit of detection close to 5×10?9 mol L?1 (with preconcentration for 60 s). The method capable to determine Os(IV) in the presence of both Pt(IV) and Ir(III) was tested on model solutions as well as with real sample of industrial waste water (spiked with the analyte); both yielding the recovery rates within 88–99%. 相似文献
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9.
Shkumbatiuk R Bazel YR Andruch V Török M 《Analytical and bioanalytical chemistry》2005,382(6):1431-1437
A new, simple, rapid, and sensitive spectrophotometric method has been developed for the determination of nitrophenols [picric acid (PA); dinitrophenols (DNP)] in wastewater samples. The method is based on the reaction of nitrophenols with 2-[(E)-2-(4-diethylaminophenyl)-1-ethenyl]-1,3,3-trimethyl-3 H-indolium chloride reagent to form the colored ion associates, which are extracted by organic solvents. The molar absorptivity of the ion associates of PA with the investigated reagent ranges from 8.3×104 to 11.3×104 L mol–1 cm–1, depending on the extractant. Because only PA is extracted in an acidic medium with the investigated reagent, but both PA and DNP are extracted in an alkaline medium, it is possible to determine both substances in a mixture. Appropriate reaction conditions have been established. The absorbance of the colored extracts obeys Beers law in the range of 0.04–4.58 mg L–1 PA, 1.0–18.4 mg L–1 2,4-DNP and 1.2–14.7 mg L–1 2,6-DNP, respectively. The limit of detections, calculated from a blank test (n=10; P=0.95), are 0.05 mg L–1 PA, 0.9 mg L–1 (2,4-DNP), and 1.1 mg L–1 (2,6-DNP), respectively. 相似文献
10.
建立了散射背景下测定人体血清中Zn^2+含量的激光热透镜光谱分析方法。比较了蛋白质微粒散射对于分光光度法和激光热透镜光谱分析法测定的影响。结果表明,激光热透镜光谱分析方法能够避免溶液中存留蛋白质微粒散射的影响。Zn^2+量在0~1.6μg/mL范围内呈线性关系(r=0.9986),检出限为1ng/mL。应用于人体血清中Zn^2+含量的测定,与原子吸收法测定结果基本一致。 相似文献