Study On Quality Standard Of Piperazinylethylisoflavones Ether And Isoflurane Injection

Piperazinylethylisoflavones ether is a new synthesized compound that can be used for the prevention and treatment of osteoporosis and other disease caused by osteoporosis.For further study on this substance, in this article, the structure of Piperazinylethylisoflavones ether was analyzed and the main characteristic adsorption bands in its IR spectral and fragment ions in its mass spectral are also assigned by using a series of spectral techniques including UV, IR, MS, NMR and the element analysis. Especially, several kinds of 2D-NMR techniques (e. g. 1H-NMR, 13C-NMR, DEPT-13C-NMR, 1H-1HCOSY, HMQC, HMBC), which can provide valuable information, are used for confirmation of the assignment of its highly overlapping 1H-NMR and 13C-NMR signals. The combination of these techniques is applicable for the structural establishment of Piperazinylethylisoflavones ether.In addition, in this article, the quality standard of Piperazinylethylisoflavones ether was also studied: (1)ODS column as stationary phase, methanol and a mixture of 0. 025mol/L sodium phosphate monobasic and 0. 04mol/L sodium dedecyl sulfate(80:20) (adjusted with phosphoric acid to a pH 4.8) as mobile phase , 248. 6nm as detective wavelength to establish ion-pair HPLC method for the content determination and limit test of the relative substance. This established method of the relative substance limit test had good specification, linearity and precision within the range of 2. 08~8. 32ug/ml (r=0. 9999), the limit of detection is 0.2ng(S/N=3).The established content method had good linearity within the range of 19.7 ~ 78. 8ug/ml(r=0. 9999). The RSD with-in day and between-day were 0.30% and 0.96%, respectively. (2)Anhydrous acetic acid as solvent, 0.1mol/L perchloric acid as titrant, potentio-metric method indicating end-piont to establish non-aqueous titration method for determination of Piperazinylethylisoflavones ether. The established method is simple, accurate and precise. The RSD with-in day and between-day were 0.34% and 0.32%, respectively. (3)Silica GF254 as adsorptive reagent ; toluene-methanol (4:1) as the developer; chamber saturated with the developer and ammonia to establish the TLC method for the relative substance of Piperazinylethylisoflavones ether. (4) For the limit test of residual solvent in Piperazinylethylisoflavones ether drug substance, A capillary GC method was established using HP-1 (30m×0.53mm×0.33 μm) as the analytical column; 3mX0. 53mm fused silica capillary column as the guard column; nitrogen as the carrier gas with a flow rate of 20ml/min; the flow rate of air and hydrogen was 250ml/min and 35ml/min; the oven temperature held at 100℃; The injector anddetector temperatures were maintained at 220°C and 250°C; The split ratio was 1:1.The method had a good specification and sensitivity.(二) STUDY ON QUALITY STANDARD OF ISOFLURANE INJECTION At present, isoflurane is used widely as a sort of volatile general anesthetics. In the traditional way, isoflurane was presented into respiratory tract by respiration machine . With the development of general anesthetics, isoflurane can be injected directly into vein. In this article,we established a method for determination of isoflurane and its related substances in isoflurane injection. The isoflurane injection was dissolved with n-butanol, and then detected by capillary gas chromatograph. N-hexane was used as the internal standard. The linear range of determination of related substances was 60~ 180ug/ml.The regression equation was Y=0.0086X+0.0018 (r=0. 9996). The limit of detection was 60ng. The linear range of determination of isoflurane injection was 6 ~ 18mg/ml. The regression equation was Y=0.1035X-0.0023 ( r=0.9999). The average recoveries of the method was 99. 49%, RSD=1.1%. The RSD of the inter-day and intra-day variation were 0. 48% and 0. 87%, respectively. The method was simple, selective and reproducible for the assay of isoflurane in isoflurane injection.