Thesis (Ph.D.)--Michigan State University. Dept of Chemistry, 2006. / Title from PDF t.p. (viewed on June 19, 2009) Includes bibliographical references. Also issued in print.

Thesis (M.S.)--Rochester Institute of Technology, 1981. / Typescript. Includes bibliographical references (leaves 83-84).

Thesis (M.S.)--Rochester Institute of Technology, 1990. / Spine title: Chromatographic retention and donor and acceptor numbers. Typescript. Includes bibliographical references.

Thesis (Ph.D.)--Virginia Commonwealth University, 2009. / Prepared for: Dept. of Chemistry. Title from title-page of electronic thesis. Bibliography: leaves 144-153.

Thesis (M.S.)--University of Wisconsin--Madison, 1966. / eContent provider-neutral record in process. Description based on print version record. Includes bibliographical references (leaves 34-36).

Thesis (Ph. D.)--University of Florida, 1989. / Description based on print version record. Typescript. Vita. Includes bibliographical references (leaves 231-243).

Thesis (Ph. D.)--University of Washington, 1981. / Vita. Bibliography: leaves [131]-135.

Made available in DSpace on 2014-10-09T12:23:26Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:56:17Z (GMT). No. of bitstreams: 1 01286.pdf: 650090 bytes, checksum: 1ebec3348e6667e7f920bd6f26ab213e (MD5) / Dissertacao (Mestrado) / IEA/D / Faculdade de Medicina, Universidade de Sao Paulo - FM/USP

The development of the monograph of a commonly used Chinese medicine, Lini Semen, for the Hong Kong Chinese Materia Medica Standards (HKCMMS) was recorded. HKCMMS is a set of reliable and internationally recognized standards of Chinese medicine. The monograph of Lini Semen was proposed, endorsed, and under editorial phase for the publication of the 9th volume of HKCMMS. In the proposed HKCMMS monograph of Lini Semen, besides regular content such as macroscopic and microscopic identification, and TLC identification, a HPLC fingerprint method and two assay methods were developed. All methods were well-established and validated. TLC identification: Lini Semen n-hexane extract is identified on a HPTLC Silica gel RP-18 plate, with α-linolenic acid and linoleic acid as the markers. The developing system consisted of acetone, acetic acid and dichloromethane in the ratio of 5:4:2. The spraying reagent was 5% sulphuric acid - ethanol solution and the plate was observed under 366 nm. HPLC fingerprint: Fingerprint of Lini Semen was conducted on a HPLC system with a C8 column. Mobile phase consisted of (A) water and (B) acetonitrile and isopropanol (9:1). Six characteristic peaks, including α-linolenic acid and linoleic acid were detected under 210 nm. Assay: α-Linolenic acid and linoleic acid were detected from Lini Semen n-hexane extract under the same HPLC condition of the fingerprint of Lini Semen. The proposed total content of α-linolenic acid and linoleic acid was not less than 0.56%. Secoisolariciresinol diglucoside (SDG) was detected from hydrolysed Lini Semen extract by HPLC system with a C18 column. Mobile phase consisted of (A) water and (B) acetonitrile. The detection wavelength was 280 nm. The proposed content of SDG was not less than 0.81%. Conclusion: It is the first time to propose a HPLC fingerprint and introduce SDG as a assay marker of Lini Semen in a regional standard monograph. The established methods for TLC identification, HPLC fingerprint, assay of the total content of α-linolenic acid and linoleic acid, as well as assay for SDG were validated with in-house and inter-laboratory comparison to prove that the methods are reliable.

This project has focused on the applicability of using superheated water as an alternative eluent for use in reversed phase high performance liquid chromatography (RP-HPLC). A system based on instrumentation from gas chromatography (GC), HPLC, and supercritical fluid chromatography (SFC) was utilised with some success. Of particular importance was the stability of the column stationary phases commonly employed in RP-HPLC. The most popular phases based on alkyl bonded silica proved unsuitable due to excessive dissolution of the base silica at high temperatures. Nevertheless, two other phases—one a poly(styrene-divinylbenzene) material and the other a porous graphitic carbon—proved stable to temperatures as high as 240°C. At such temperatures compound stability was good, except for a notable case with nitrobenzene. The mechanism of elution remained reversed phase mode throughout, with polar solutes being eluted before non-polar ones.