Size exclusion chromatographic determination of hydroxypropyl methyl cellulose and polyethylene glycol 400 in an ophthalmic solution

Summary Hydroxypropyl methyl cellulose (HPMC) and polyethylene glycol 400 (PEG 400) content in HypoTears™ Daily Dose ophthalmic solution are determined simultaneously by size exclusion chromatography. The retention times of HPMC and PEG 400 are 10.6 and 15.4 minutes, respectively. The method requires minimal sample pretreatment and is accurate and reproducible. The peak area response from a refractive index detector versus HPMC and PEG 400 concentration is linear over the range of 50–150 % of their label claims of 2.5 mg/mL and 10 mg/mL, respectively. The mean absolute recoveries of HPMC and PEG 400 at their label claim using the described method are 98.9±1.3 % and 100.4±1.2 % (mean±SD, n=12), respectively.     

萃取色谱法富集原子吸收法测定环境水中超痕量金属元素──两种萃取剂的比较

本文研究并比较了分别以８－羟基喹啉和巯基苯骈噻唑为萃取剂，以活性硅胶为载体的柱式萃取色谱法对环境水中Ｚｎ、Ｃｕ、Ｐｂ、Ｃｄ、Ｆｅ、Ｃｏ、Ｎｉ和Ｍｎ的最佳富集和洗脱条件。实验证明，后者明显优于前者。以巯基苯骈噻唑为萃取剂的色谱柱对金属元素的吸附具有快速、完全、寿命长和重现性好等特点。在ｐＨ＝７～８之间回收率可达９８％以上，富集倍数为２００倍。     

高频单线圈双调谐NMR单晶探头的研制

本文报道了一种测角单晶NMR探头。该探头采用单线圃双调谐电路,工作频率在90MHz-110 MHz连续可调,可进行交叉极化大功率去耦实验。文中提出了一种简单而有效的测角装置,可使单晶绕三个互相垂直轴转动实现单晶的NMR测量。作为典型的应用例子,本文利用该探头实现了单晶DGO(2NH₂CH₂COOH·H₂C₂O₄)屏蔽张量的测量。     

The method of concentrating a substance from a solution in a stationary sorbent layer and its theoretical basis

The principle of concentrating a substance from a mixture flow in a stationary sorbent layer of infinite length that was previously developed for gas chromatography is extended to liquid chromatography. Translated fromIzevestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 1063–1065, May, 1997.     

Early Evolution of Gas Chromatography in East Germany. Part I: Beginnings, Instrument and Column Development and Organizations

The early evolution of gas chromatography in the former German Democratic Republic (GDR) is surveyed and instrument development is outlined, describing the most important models manufactured in the GDR. The organization of the Arbeitsgemeinschaft für Gas-Chromatographie (Working Group for GC) is chronicled and its activities are discussed. Subsequent parts of this article will deal with the six symposia organized by the Arbeitsgemeinschaft between 1958 and 1968.     

High-Throughput Screening of Ten Microcystins and Nodularins, Cyanobacterial Peptide Hepatotoxins, by Reversed-Phase Liquid Chromatography-Electrospray Ionisation Mass Spectrometry

Liquid chromatography-electrospray ionisation mass spectrometry was evaluated in the high-throughput analysis of microcystins and nodularins, cyanobacterial peptide hepatotoxins. Extracts originating from cyanobacterial strains and field material were separated on a 30 mm × 4 mm I.D. Merck Purospher STAR RP-18e column using a rapid gradient of aqueous formic acid and acetonitrile, ionised by electrospray technique and analysed on a Micromass Quattro II triple-quadrupole mass spectrometer operated in the selected ion recording (SIR) mode. The total analysis time per sample was 2.8 min corresponding to 514 samples a day. The system showed good robustness during a series of 320 repetitive injections of a field sample containing three major microcystins.     

Syntheses and characterization of 16‐arm star and star diblock copolymer and AB8 9‐miktoarm star copolymer via NMRP and ROP from dendritic multifunctional macroinitiators

A dendritic macroinitiator having 16 TEMPO‐based alkoxyamines, Star‐16 , was prepared by the reaction of a dendritic macroinitiator having eight TEMPO‐based alkoxyamines, [G‐3]‐OH , with 4,4′‐bis(chlorocarbonyl)biphenyl. The nitroxide‐mediated radical polymerization (NMRP) of styrene (St) from Star‐16 gave 16‐arm star polymers with PDI of 1.19–1.47, and NMPR of 4‐vinylpyridine from the 16‐arm star polymer gave 16‐arm star diblock copolymers with PDI of 1.30–1.43. The ring‐opening polymerization of ε‐caprolactone from [G‐3]‐OH and the subsequent NMRP of St gave AB₈ 9‐miktoarm star copolymers with PDI of 1.30–1.38. The benzyl ether linkages of the 16‐arm star polymers and the AB₈ 9‐miktoarm star copolymers were cleaved by treating with Me₃SiI, and the resultant poly(St) arms were investigated by size exclusion chromatography (SEC). The SEC results showed PDIs of 1.23–1.28 and 1.18–1.22 for the star polymers and miktoarm stars copolymers, respectively, showing that they have well‐controlled poly(St) arms. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 1159–1169, 2007.