| The quality of the Chinese medicine preparations concerns human healthy and the quality of life. With the exposure of security problem, our country has strengthened the research to the quality of Chinese medicine preparations. Due to the requirement of development of modernization and internationalization of Chinese medicine preparations, based on investigation status at present, active ingredients in Chinese patent medicine were investigated, five new methods for analysis of Chinese medicine preparations quality have been established by optimizing conditions for extracting procedure and introducing new pretreatment technologies and designing test conditions. The precise, simple and convenient methods have proved of actual application value. The dissertation constitutes with six chapters and primary coverage is as follows:(1) Based on the literature research, latest progress and research status of the quality standard, effective components, pretreatment technology and detection technology of traditional Chinese medicine preparations are summarized.(2) A high performance liquid chromatagraphy(HPLC) method was established for simultaneous determination of paeoniflorin, 1iquiritin and cinnamic acid in Yangyin Qingfei Particles using switching UV wavelength. Paeoniflorin, 1iquiritin and cinnamic acid were separated on a ZORBAX SB-C18 column with the mobile phase composed of 0.2% phosphoric(A) and acetonitrile(B) in gradient elution(0-4 min, 18%Bâ†'18%B, 4-9 min, 18%Bâ†'37%B, 9-16 min, 37%Bâ†'37%B). Detection wavelengths were set as follows: 0-6.3 min, 276 nm, 6.3-7.3 min, 230 nm, 7.3-16 min, 276 nm. The column temperature was maintained at 28℃. The flow rate was at 1.0 m L·min-1. The calibration curves of paeoniflorin, 1iquiritin and cinnamic acid showed good linearity within 0.2368-4.736, 0.1708-3.416 and 0.0352-0.704 μg·m L-1, respectively. The average recoveries of these were 99.7%, 98.8% and 98.4%, respectively.(3) An effective HPLC method has been developed to simultaneously determine 1iquiritin and cinnamic acid in Jianwei Zixue Oral Solution. Chromatographic separation was achieved on a Kromasil C18 column with the mobile phase composed of 0.2% phosphoric(A) and acetonitrile(B) under the condition of gradient elution(0-6 min, 26%Bâ†'45%B, 6-9.5 min, 45%Bâ†'90%B, 9.5-10 min, 90%Bâ†'95%B) at a flow rate of 1.0 m L·min-1. The UV detection was at 276 nm. The column temperature was 28℃. A good linearity response was obtained for 1iquiritin and cinnamic acid in the concentration range of 0.7676-38.38 and 0.04288-2.144 μg·m L-1, respectively. The average recoveries were 98.4% and 98.9%, respectively.(4) A method combining solid-phase extraction(SPE) and HPLC has been established to simultaneously determine paeoniflorin, ferulic acid and paeonol in Fufang Wuji Granules. The technics parameters including chromatographic column types, proportion and acidity of mobile phase, extraction solvent, extraction time and eluting solvent types, elution solvent types and elution solvent volumes of solid phase extraction were optimized. The sample was extracted in ultrasonic bath, then purified and concentrated with HYPERSEP Retain-PEP cartridge. The extract was separated on Kromasil C18(250 mm × 4.6 mm, 5 μm) by gradient elution(0-4 min, 22%Bâ†'22%B, 4-5 min, 22%Bâ†'30%B, 5-8 min, 30%Bâ†'45%B, 8-9 min, 45%Bâ†'59%B, 9-13 min, 59%Bâ†'69%B) using 1.0% phosphoric acid(A) and acetonitrile(B) as mobile phase, which was detected at 230 nm for paeoniflorin in 0-8 min, 321 nm for ferulic acid in 8-10 min and 274 nm for paeonol in 10-15 min. The column temperature was at 28℃. The flow rate was 1.0 m L·min-1. The calibration curves of aeoniflorin, ferulic acid and paeonol showed good linearity within 3.12-312, 0.246-24.6 and 0.0896-8.96 μg·m L-1, respectively. The average recoveries were 98.6%, 96.3% and 99.9%, respectively.(5) To simultaneously determine paeoniflorin, 1iquiritin, baicalin and costunolide in Fuke Yangkun Pills, a HPLC method has been developed. Response surface methodology(RSM) was utilized to forecast the optimum extraction technology. Separations of target compounds were performed on Kromasil C18(250 mm × 4.6 mm, 5μm). The mobile phase consisted of 0.2% phosphoric acid(A) and acetonitrile(B) at a flow of 1.0 m L·min-1 in a gradient profile as follows: 0-6 min, 23%Bâ†'23%B, 6-7 min, 23%Bâ†'25%B, 7-12 min, 25%Bâ†'80%B, 12-13 min, 80%Bâ†'95%B. Switching UV wavelength procedure(0-6 min, 230 nm, 6-8 min, 276 nm, 8-13 min, 280 nm, 13-17 min, 225 nm) was applied. The column temperature was at 28℃. These ingredients have higher linearity in 1.616-161.6, 0.4318-43.18, 1.3248-132.48 and 0.5184-51.84 μg·m L-1, respectively. Recoveries measured of paeoniflorin, 1iquiritin, baicalin and costunolide were 97.5%, 99.7%, 96.3% and 97.0%, respectively.(6) A novel method for determination gallic acid, rhein and emodin in Fufang Xiaozhi Suppository by HPLC coupled with SPE was proposed. The sample was purified and enriched by HYPERSEP C18 cartridge. The HPLC system included Kromasil C18(250 mm × 4.6 mm, 5 μm) and the mobile phase composed of 0.5% phosphoric acid(A) and acetonitrile(B) with gradient elution(0-4 min, 22%Bâ†'22%B, 4-5 min, 22%Bâ†'30%B, 5-8 min, 30%Bâ†'45%B, 8-9 min, 45%Bâ†'59%B, 9-13 min, 59%Bâ†'69%B) at a flow rate of 1.0 m L·min-1. The detection wavelength was 273 nm for gallic acid and 254 nm for rhein and emodin, respectively. The column temperature was at 28℃. The linear ranges of these were 0.2964-14.82, 0.215-10.75 and 0.3072-15.36 μg·m L-1, respectively. Average recoveries of these were 95.1%, 95.9% and 97.8%, respectively. |
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