Studies On Chemical Constituents And Solid Dispersion Of C21 Steroidal Glycoside Degradation Products From Marsdenia Tenacissima

Cancer is a serious hazard to human health disease, cancer tumor multidrug resistance is the main reason is difficult to cure. Multidrug resistance (Multidurg Rresistance, MDR), the phenomenon seriously affect the efficacy of chemotherapy for cancer. Cancer drugs to overcome MDR, restore the sensitivity of drug resistant tumors, looking for efficiency and low toxicity of MDR reversal agents of tumor cells in cancer therapy is currently a hot research.Marsdenia Division, Department of dill japonica Asclepiadaceae Genus milk through light scattering Marsdenia tenacissima (Roxb.) Wight et Arn.’s Dried cane, its agents Xiaoaiping used in the clinical treatment of gastric cancer, lung cancer and liv er cancer and other advanced malignancy is effective. Activity Index used by our group under the direction of separation of anti-tumor effect Marsdenia material basis, to determine Marsdenia degradation products of C21 steroidal glycosides on human gastric cancer cell line SGC-7901 significantly inhibited value. Speculated Marsdenia agents Xiaoaiping reversed cancer patients and their clinical efficacy and more to drug resistance to drugs, so our group isolated and identified the use of modern tec hnology for the chemical composition of degradation products provide the material basis; by high performance liquid chromatography-evaporative light scattering detection (HPLC-ELSD) Determination of the content of the four aglycones to provide quality standards; To improve the bioavailability of solid dispersion was prepared, the establishment of Marsdenia degradation products of C21 steroidal glycosides Determination of the dissolution of solid dispersion method.Isolation and identification of the use of modern technology, from Marsdenia C21 steroidal glycosides isolated degradation products of different structures C21 ster oidal aglycones and their derivatives with different substituents in 22 (12 new compounds), their structures were: tenacigeninA (TGTHD 1); 12β-O -acet y1-tenacigeninA (TGTHD 2); 12β-O-2-methylpropionyl-tenacigenin A (TGTHD 3); 12β-O-tigloy1-tenacigenin A (TGTHD 4); 12β-O-2-methyl butyryl-tenacigenin A (TGTHD 5); tenacigenin B (TGTHD 6) lla,12β-O-diac etyl-tenacigenin B (TGT HD 7);11a-O-tigloyl-12β-O-acetyl-tenacigeninB (TGTHD 8);11a-O-2-methylp ropionyl-12β-O-acetyl-tenaci genin B(TGTHD 9); 11a-O-2-methylbutyryl-12β-O-a cetyl-tenacigenin B (TGTHD 10); 11a,12B-O-ditigloy1-tenacigenin B(TGTHD 11); 11a-O-2-methylpropionyl-12β-O-tigloyl-t enacigenin B (TGTHD 12); 11a-O-benz oy1-12β-O-t igl oyl-tenacigenin B (TGTHD 13); 11a-O-tigloyl-12β-O-be nzoyl-t enac igenin B (TGTHD 14); 11a-O-2-methylbutyryl-12β-O-tigloyl-tenacigenin B (TGTHD 15); 11a-O-2-methylbutyryl-12β-0-3-hydroxy1-2-methylenebutyry-tenacigenin B (TGTHD 16); 11a,12β-O-dibenzoyl-tenacige ninB (TGTHD 17); 11a,12β-O-di-2-methylbutyryl-tenacigenin B (TGTHD 18); 11a-O-2-methylb utyryl-12β-O-benzoyl-tenacigenin B(TGTHD 19); 11a-0-2-methylbutyryl-17β-tenaigenin B (TGTHD 20); 11a-O-tygl oyl-12β-O-benzoyl-17β-tenacigeninB (TGTHD 2 1);11a-O-2-methylbutyryl-12β-O-benzoyl-17β-te nacigenin B(TGTHD 22); 12 new compounds which were:TGTHD 3、TGTHD 4, TGTHD 9、TGTHD 12、TGTHD 13、TGTHD 14、TGTHD 16、TGTHD 17、TGTHD 18、TGTHD 20、TGTHD 21�'�TGTHD 22。In this reseach, we prepared four Marsdenia C21 steroidal glycoside degradation products reference substance, and adopted the HPLC-ELSD method for the purity determination.The study showed that each reference substances represented only one main peak by using different mobile phase; there were not unusual when changing the column and mobile phase peaks; determination consistent with the reference standard requirements. which were in accordance with the determination requirement.In this research, we determined content of Marsdenia C21 steroidal glycoside content of degradation products by HPLC-ELSD method. Investigated the effects of mobile phase on the separation and we selected HPLC conditions: column, Hypersil C6H6 (250 mm x 4.6 mm,5μm), according to Little Analytical Instruments Co., Ltd. Dalian; mobile phase:0 min (A 30%, B 70%)�'30min (A 30%, B 70%)�'40 min (A 35%, B 65%)�'75 min (A 35%, B 65%); flow rate:1.0ml.min-1; column temperature:25℃; drift tube temperature:105℃; atomization gas flow rate:3.2 L.min-1; detection device: ELSD 2000ES evaporative light detector. Linear relations, repeatability, reproducibility, stability, and recovery study methodology were conducted.In this research, we determined the dissolution of solid dispersion of Marsdenia C21 steroidal glycoside content of degradation products by HPLC-ELSD method. Chromatographic conditions were column:Hypersil C6H6 (250 mm x 4.6 mm,5μm), according to Little Analytical Instruments Co., Ltd. Dalian; mobile phase:0 min (A 30%, B 70%)�'30min (A 30%, B 70%)�'40 min (A 30%, B 70%); flow rate: 1.0ml/min-1; column temperature:25℃; drift tube temperature:105℃; atomization gas flow rate:3.2 L. min-1; detection device:ELSD 2000ES evaporative light detector. Specificity tests, linear relations, precision, reproducibility, stability, recovery rate, uniformity and reproducibility study methodology were conducted.