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71.
Trace analysis of rapamycin in human blood by micellar electrokinetic chromatography 总被引:1,自引:0,他引:1
A capillary electrophoretic method with UV detection at 278 nm has been developed for analysis of the immunosuppressant rapamycin (sirolimus) in human blood at low microgram per liter levels. Separation has been achieved in an acidic carrier electrolyte containing sodium dodecylsulfate and 30% (v/v) acetonitrile. For sample clean-up and preconcentration, an off-line solid-phase extraction step using a silica-based reversed-phase material and an on-capillary focussing technique were employed. The latter allows the injection of increased sample volumes without excessive band broadening. Although this new method is less sensitive than existing liquid chromatographic procedures combined with mass spectrometry, it is fully suited to routine analysis of rapamycin in blood from patients treated with this drug. Last but not least the low costs make it an attractive alternative to established methods. 相似文献
72.
Blends of ABS (acrylonitrile–butadiene–styrene) with phenoxy(poly(hydroxyether bisphenol A)) were prepared using a Branender single screw extruder. Scanning and transmission electron micrographs (SEM, TEM) showed a typical two-phase morphology; particle-in-matrix (90/10) (ABS/phenoxy by weight), 70/30, 10/90), island/sea (30/70) and co-continuous (50/50) morphologies. The glass transition temperature (Tg) of SAN was almost unchanged in the blends, while the Tg of phenoxy increased by about 5 °C in the blends. The synergistic effect of tensile modulus and strength was noted in ABS-rich blends, where a drastic drop of ductility was seen, and the results were interpreted in terms of rubber particle migration form SAN to phenoxy phase, which was visualized by TEM. Melt viscosity showed yield in ABS-rich blends, and generally followed the log additivity. 相似文献
73.
74.
Anzalone PW Baru AR Danielson EM Hayes PD Nguyen MP Panico AF Smith RC Mohan RS 《The Journal of organic chemistry》2005,70(6):2091-2096
[reaction: see text] Three one-pot methods for the conversion of aldehydes to homoallyl ethers catalyzed by Bi(OTf)(3).xH(2)O (1 < x < 4) have been developed. The one-pot synthesis of homoallyl ethers can be achieved either by in situ generation of the acetal followed by its reaction with allyltrialkylsilane or by a three-component synthesis in which the aldehyde, trimethylorthoformate or an alkoxytrimethylsilane and allyltrimethylsilane are mixed together in the presence of bismuth triflate (0.1-1.0 mol %). In addition, a three-component synthesis of homoallyl acetates, which is achieved by reacting the aldehyde, acetic anhydride, and allyltrimethylsilane in the presence of bismuth triflate (3.0-5.0 mol %), has been developed. The use of a relatively nontoxic, easy to handle, and inexpensive catalyst adds to the versatility of these methods. 相似文献
75.
Chi -ping Lau 《manuscripta mathematica》1987,59(1):53-62
It is shown that if the order of non-uniformity of a quasi-linear elliptic equation is h,1
0,2(h–1)/h norm. For 0h1,existence of a bounded solution is guaranteed without any smallness assumption on the given boundary data.More precise information is given for the special case of the minimal surface equation. 相似文献
76.
Bao Gia Nguyen 《Journal of statistical physics》1987,49(1-2):235-243
A study is made of the gap exponents for percolation processes with the triangle condition in the subcritical region. It is show that the gaps are given by
t
=2 fort=2, 3,. Scaling theory predicts thatP
p
(¦C
0¦S(p))–(p
c
–p) andE
p
(1/¦C
0¦; ¦C
0¦S(p))–(p
c
–p)3, whereS(p) is the typical cluster size. It is found that (p
c
–p)P
p
(|C
0S(p)
1–)(p
c
–p)1–2 and (p
c
–p)3E
p
(1/|C
0|;|C
0|S(p)
1–))(p
c
–p)3–4. 相似文献
77.
78.
Treatment of (thd)H (thd=2,2,6,6-tetramethyl-3,5-heptandionate) with excess Os3(CO)12 in an autoclave at 180°C gives the formation of a brown metal chain complex [Os2(CO)5(thd)2]2 (1) and a yellow CO2 cluster complex [Os4(-H)(-CO2)(thd)(CO)13] (2) in low yields. Complex 2 was fully identified by a combination of spectroscopic methods and X-ray diffraction study, showing a unique CO2 ligand bridging a triosmium metal fragment, Os3(-H)(CO)10 and a monometallic osmium fragment, Os(CO)3(thd). Upon treatment of 1 with Me3NO at an elevated temperature, oxidation of the CO ligand occurred at the position trans to the unique CO2 ligand on the Os(CO)3(thd) fragment, giving the formation of a second CO2 cluster [Os4(-H)(-CO2)(thd)(CO)12(NCMe)] (3), which is stabilized by a weakly coordinated acetonitrile molecule. 相似文献
79.
80.
The keto-enol tautomerization of p-hydroxyphenylpyruvic acid (pHPP) in aqueous solutions and the complexation reaction between enolic pHPP and boric acid have been studied by electrochemical techniques including linear sweep voltammetry (LSV), pulse voltammetry, and cyclic voltammetry (CV), combining with UV spectrometry. Electrochemical techniques reveal that in aqueous solution, there are two tautomers of pHPP: enolic form and ketonic form; the former exists mainly in freshly prepared pHPP solution, and the latter exists mainly in equilibrium solution. Both enolic and ketonic pHPP are electroactive. The electrochemical oxidation of enolic pHPP gives rise to two anodic waves, I(a) and II(a), while the electrochemical oxidation of ketonic pHPP only results in the observation of the second wave II(a). The oxidation process I(a) is revealed to be associated with the quasi-reversible, two-electron two-proton oxidation of "C=C"group at the side chain of enolic pHPP, and the oxidation process II(a) is proposed to result from the irreversible oxidation of phenolic hydroxyl group. It is observed that in aqueous solution, enolic pHPP can quickly complex with boric acid to yield enol-borate complex that can also oxidize at a glassy carbon electrode to yield an anodic wave. 相似文献