Study On Structure And Quality Standard Of PM Disodium Salt

PM Disodium Salt is a new synthesized compound that can be used for central anesthesia .For further study on this substance,in this article,the structure of PM Disodium Salt 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.The combination of these techniques is applicable for the structural establishment of PM Disodium Salt.In addtion, in this article,the quality standard of PM Disodium Salt was also studied: (1)ODS column as stationary phase,methanol-water-15%TBAH(70: 22: 8) ( phosphoric acid adjusts with pH of moblie phase to be 6.0) as mobile phase,263nm 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 42.0～201.0ng (r = 0.9994),the limit of detection is 0.9ng (S/N=3) .The established content method had good linearity within the range of 0.81～4.01μg (r = 0.9999).The RSD within in-day and between-day were 0.21 %,0.11% respectively. (2)Water as solvent, 0.05mol/L Hydrochloric Acid as titrant, bromophenol blue indicating end point to establish titration method for determination of PM Disodium Salt. The established method is simple, accurate and precise. The RSD within in-day and between-day were 0.0090 %及0.025 % respectively. (3) ODS column as stationary phase, methanol-water (75: 25) as mobile phase, 270nm as detective wavelength to establish HPLC method for limit test of PPF .This established method of PPF limit test had good specification, linearity and precision within the range of 6. 69—322. 5ng (r = 0.9999), the limit of detection is 0.018ng( S/N= 10). (4) For the limit test of residual solvent in PM Disodium Salt, capillary GC method was established, the method had good specification and sensitivity. Chromatographic condition: use HP-20M(30m×0.53mm×1.33μm) as the analitical column; Helium as the carrier gas with a flow rate of 20ml/min; the flow rates of air and hydrogen were 300ml/min and 40ml/min; the oven . temperature uses a programmable temperature as follows: 33℃2min, then20℃/min to 60℃10min; The injector and detector temperatures were both maintained at 200°C; The split ratio was 1: 1; Helium was used ast he makeup at 15ml/min.The quality standard of PM Disodium Salt injection was also studied, the method was in accordance with the crude drug.