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61.
Li AC Alton D Bryant MS Shou WZ 《Rapid communications in mass spectrometry : RCM》2005,19(14):1943-1950
Bioanalytical support of plasma pharmacokinetic (PK) studies for drug discovery programs primarily involves the quantitative analysis of dosed compounds using liquid chromatography/atmospheric pressure ionization tandem mass spectrometry (LC/MS/MS) operated in selected reaction monitoring (SRM) mode. However, there is a growing need for information on the metabolism of new chemical entities (NCEs), in addition to the time-concentration profiles from these studies. In this paper, we present a novel approach to not only quantify parent drugs with SRM, but also simultaneously screen for metabolites using a hybrid triple quadrupole/linear ion trap (QqQ(LIT)) instrument. This was achieved by incorporating both the conventional SRM-only acquisition of parent compounds and the SRM-triggered information-dependent acquisition (IDA) of potential metabolites within the same scan cycle during the same LC/MS/MS run. Two test compounds were used to demonstrate the applicability of this approach. Plasma samples from PK studies were processed by simple protein precipitation and the supernatant was diluted with water before injection. The fast scanning capability of the linear ion trap allowed for the information-dependent acquisition of metabolite MS/MS spectra (<1 s/scan), in addition to the collection of adequate data points for SRM-only channels. The MS/MS spectra obtained from potential metabolites in post-dose samples correlated well with the spectra of the parent compounds studied, therefore providing additional confirmatory structure information without the need for repetitive analyses. Relative quantitative time-concentration profiles of identified metabolites were also obtained. Furthermore, this articulated SRM+SRM-IDA approach generated equivalent quantitative results for parent compounds to those obtained by conventional SRM-only analysis. This approach has been successfully used to support discovery PK screening programs. 相似文献
62.
An operationally simple oxidative methyl esterification of primary alcohols in good yields using an iodine‐mediated poly[4‐(diacetoxyiodo)styrene] in methanol at room temperature is described. The polymeric reagent can be regenerated and reused as an environmentally benign reagent. 相似文献
63.
本文给出时空流形的一种简化的旋量描述形式。特别是证明了在Newman-Penrose方程中有六个多余的方程。作为对杨振宁引力场方程的应用,求得全部O型和一部分N型“纯粹空间”。 相似文献
64.
Yu Rong Ren Shu Yong Jia Shou Cai Zhang Chun Ling Liu Yun Cheng Cui 《中国化学快报》2007,18(7):872-874
Stannous oxalate was prepared efficiently and characterized by XRD and FT-IR. It exhibited higher catalytic activity and had profitable effect than tetrabutyl titanate and stannous octoate for the synthesis of polytrimethylene terephthalate (PTT) via esterification-route. Over this catalyst, the degree of esterification of pure terephthalic acid was up to 94.4% at 260°C after 1.5 h, while the intrinsic viscosity and content of terminal carboxyl groups of the corresponding PTT polyester, polymerized at 260°C, 60 Pa for 2 h, was 0.8950 dL/g and 15 mol/t, respectively. Stannous oxalate was a promising catalyst for the synthesis of PTT polyester. 相似文献
65.
采用多拷贝同时搜寻法(MCSS), 并结合现有微管抑制剂的SAR及3D-QSAR对β微管蛋白中Taxol(紫杉醇)结合腔的性质进行了分析. 结构研究结果表明, Taxol结合腔以疏水性质为主, 并指出官能团分布的具体位置: 在Phe270上方(Leu361-Pro272-Leu273-Leu228之间)的弧形区域、Asp26羧基下方及其与Glu22羧基之间、M-loop的中部, 以及Asp224内侧且靠近Arg276的胍基的位置. 而Asp224的内侧又是新提出的结合位点. 研究结果符合现有微管抑制剂的SAR, 为现有抗肿瘤药物的结构改造以及小分子微管抑制剂设计提供了理论依据. 相似文献
66.
67.
A piezoelectric method is proposed for the determination of sulfite in concentration range 1 × 10–7–1 × 10–5 mol/1. The method is based on the redox reaction of sulfite with iodine followed by measuring frequency change of the piezoelectric crystal caused by the unreacted iodine. The method is applied to the determination of sulfite in liquor. 相似文献
68.
Addition of one equivalent of LiN(i-Pr)2 or LiN(CH2)5 to carbodiimides, RN=C=NR [R=cyclohexyl (Cy), isopropyl (i-Pr)], generated the corresponding lithium of tetrasubstituted guanidinates {Li[RNC(N R^′2)NR](THF)}2 [R=i-Pr, N R^′2=N(i-Pr)2 (1), N(CH2)5 (2); R=Cy, N R^′2=N(i-Pr)2 (3), N(CH2)5 (4)]. Treatment of ZrCl4 with freshly prepared solutions of their lithium guanidinates provided a series of bis(guanidinate) complexes of Zr with the general formula Zr[RNC(N R^′2)NR]2Cl2 [R=i-Pr, N R^′2=N(i-Pr)2 (5), N(CH2)5 (6); R=Cy, N R^′2=N(i-Pr)2 (7), N(CH2)5 (8)]. Complexes 1, 2, 5-8 were characterized by elemental analysis, IR and ^1H NMR spectra. The molecular structures of complexes 1, 7 and 8 were further determined by X-ray diffraction studies. 相似文献
69.
Polymer-supported reagents for organic synthesis are enjoying a renewed popularity with the emergence of combinatorial chemistry in recent years1. 4-(Arylseleno)morpholines formed in situ are useful -seleno-introducing reagents for saturated aldehydes2. -Sele- noaldehydes, as a frequently used intermediates, can be converted into -haloaldehydes by halogenating reaction3. However, organic selenium reagents always have a foul smell and are quite toxic, which is often problematic in organic sy… 相似文献
70.
研究了1-正-辛基-3,3-二甲基-吲哚啉-2,2′-螺-5′,6′-(2-溴-4-硝基-苯并)吡喃, 1-正-辛基-3,3-二甲基-吲哚啉-2,2′-螺-5′,6′-(4-硝基-苯并)吡喃, 1-正-辛基-3,3-二甲基-吲哚啉-2,2′-螺-5′,6′-(2,4-二硝基-苯并)吡喃及1-正-辛基-3,3-二甲基-吲哚啉-2,2′螺-5′6′-(2-氯-4-硝基-苯并)吡喃在环已烷和甲苯溶液中光致开环过程的瞬态吸收光谱。观察到具有较长寿命的中间体及聚集体的存在。初步提出异构化反应过程的机制中既包含有三重态过程, 也有单重态参与。 相似文献