Study On The Improvement Of Quality Standard Of Semen Ziziphi Spinosae, Ligustrum Lucidum And Schisandra Chinensis

Ziziphi Spinosae Semen, Ligustri Lucidi Fructus and Schisandrae Chinensis Fructus are common used Chinese herbal medicines. Quality standards of decoction pieces of Ziziphi Spinosae Semen, baked Ziziphi Spinosae Semen, Ligustri Lucidi Fructus, wine-baked Ligustri Lucidi Fructus, Schisandrae Chinensis Fructus and vinegar-baked Schisandrae Chinensis Fructus were recorded in Chinese Pharmacopoeia (version of 2010). As the index components of quality standard are simple, pretreatment content were complicated, time-consuming and low efficiency. In addition, the index components were lack of date supporting with water decoction of common clinical.Aimed at the shortcomings, it needed to be further improved. By taking the legal decoction pieces of Semen Ziziphi Spinosae, Ligustrum lucidum, Schisandra chinensisa as the study objects in this paper, added C18 TLC identification, established fingerprint and content determination of multi-index components, and on the basis, studied the decoction pieces and compound decoction in order to improve the quality control level of their quality standards.1. Improved method of TLC identification of Chinese PharmacopoeiaThe TLC identification of six herbal pieces was improved. The study of TLC simplified pretreatmen method of samples and increased index components of qualitative identification. It could save detection time and cost, and improve detection efficiency.2. Established method of TLC identification by C18 TLCThe TLC identification of seven herbal pieces was established by using C18 TLC for the first time. The study of C18 TLC increased the index components, enriched the information of qualitative identification of pieces; the C18 TLC reported basically the same result as HPLC, and had low-toxic solvent, advantages of easy operation, short analysis time and large amount of analysis. C18 TLC could be used for rapid and high throughput detection for herbal pieces.3. Established HPLC fingerprintThe HPLC fingerprints of Ziziphi Spinosae Semen, baked Ziziphi Spinosae Semen, Ligustri Lucidi Fructus, wine-baked Ligustri Lucidi Fructus, Schisandrae Chinensis Fructus and vinegar-baked Schisandrae Chinensis Fructus were established. There were 14 characteristic peaks in the fingerprint of Ziziphi Spinosae Semen and baked Ziziphi Spinosae Semen; there were 17 characteristic peaks in the fingerprint of Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus; there were 13 characteristic peaks in the fingerprint of Schisandrae Chinensis Fructus and vinegar-baked Schisandrae Chinensis Fructus. The reference fingerprint of Ziziphi Spinosae Semen, baked Ziziphi Spinosae Semen, Ligustri Lucidi Fructus, wine-baked Ligustri Lucidi Fructus, Schisandrae Chinensis Fructus and vinegar-baked Schisandrae Chinensis Fructus were established by using the Traditional Chinese medicine fingerprint similarity evaluation software.The HPLC-ESI-MS/MS was used to identify the chemical constituent of main characteristic peaks in the fingerprints. There were 16 characteristic peaks of the fingerprint of Ziziphi Spinosae Semen and baked Ziziphi Spinosae Semen were identified. There were 17 characteristic peaks of the fingerprint of Ligustri Lucidi Fructus, wine-baked Ligustri Lucidi Fructus were identified. There were 11 characteristic peaks of the fingerprint of Schisandrae Chinensis Fructus and vinegar-baked Schisandrae Chinensis Fructus were identified. The identification of characteristic perks made the information of the fingerprints more definitely.4. Established methods of simultaneously determination of multiple ingredientsBased on the fingerprint, multiple ingredients were simultaneously determination. The samples were tested by the method and compared the content of different components of processed products in order to put forward feasible identification indicator. The methods for content determination of spinosin, jujuboside A and jujuboside B by HPLC were established individually, the content of three components had no significant difference between Ziziphi Spinosae Semen and baked Ziziphi Spinosae Semen; the methods for content determination of salidroside, tyrosol, specnuezhenide, luteolin-7-O-glucoside, luteolin, apigenin, oleanolic acid and ursolic acid by HPLC were established individually, the content of salidroside, tyrosol, luteolin and apigenin had significant difference between Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus, luteolin and apigenin can be used for identification; the methods for content determination of schisandrin, schisandrol B, deoxyschizandrin, y-schisandrin, schisandrinC by HPLC were established individually, the content of deoxyschizandrin and y-Schisandrin had significant difference between Schisandrae Chinensis Fructus and vinegar-baked Schisandrae Chinensis Fructus and they could be used for identification.5. Compared the content of the water decoctionIn this study, combined with the actual application, compared the change of content before and after water boiled of in Ziziphi Spinosae Semen, Ligustri Lucidi Fructus, Schisandrae Chinensis Fructus, suanzaoren decoction, erzhi pills and sheng mai san by using the method of content determination already established. Three components could be detected in Ziziphi Spinosae Semen and baked Ziziphi Spinosae Semen single boiling decoction, content transfer rate:spinosin were 46%,47%, jujuboside A were 42%,48%, jujuboside B were 32%,23%. Content transfer rate of suanzaoren decoction:spinosin were 85%, jujuboside A and jujuboside B were about 50%. Salidroside, tyrosol, specnuezhenide, luteolin-7-O-glucoside could be detected in Ligustri Lucidi Fructus and wine-baked Ligustri Lucidi Fructus single boiling decoction, content transfer rate:salidroside were 107%,93%, tyrosol were 114%,100%, specnuezhenide were 89%,91%, luteolin-7-O-glucoside were 65%,46%. Content transfer rate of erzhi pills:salidroside, tyrosol and specnuezhenide were 49%,82%, 28%. Schisandrin, schisandrol B, deoxyschizandrin could be detected in Schisandrae Chinensis Fructus and vinegar-baked Schisandrae Chinensis Fructus single boiling decoction, content transfer rate:schisandrin were 83%, schisandrol B were 55%,48% deoxyschizandrin were about 3%. Five components could be detected in sheng mai san, content transfer rate:schisandrin were 11%, schisandrol B were about 7%,deoxyschizandrin, y-Schisandrin and schisandrin C were about 1%～2%. By analysing the compounds decocting information and content transfer rate, the study could provide the data support for the development of quality standard and clinical application.