摘要
目的:完善复方苯海拉明克罗米通酊的试行国家药品标准[1],增订乙醇量的GC测定法[2]和克罗米通含量的HPLC测定法,更好的控制产品质量。方法:乙醇量测定固定相采用直径为0.25mm～0.18mm的二乙烯苯-乙基乙烯苯型高分子多孔小球作为载体,柱温为190℃,FID检测器;固定相或采用固定液为100%的二甲基聚硅氧烷的毛细管柱,柱温为程序升温:60℃保持3min,再以20℃Wmin的升温速率升至250℃。样品用内标溶液(0.2%正丙醇的N,N-二甲基甲酰胺溶液)稀释,内标法定量。克罗米通含量测定色谱柱采用VenusilMP-C18柱,柱温为室温,流动相为磷酸盐缓冲液(0.05molWL磷酸二氢钾溶液,含1%三乙胺,并用磷酸调节pH值至4.0)-乙腈(60:40),流速为1mLWmin,检测波长为242nm,样品用乙醇稀释10倍后再用流动相稀释10倍,滤过后测定,外标法定量。结果:乙醇在0.3924mgWmL～5.886mgWmL的浓度范围内线性关系良好,相关系数为0.9999,高、中、低浓度平均加样回收率为99.6%,RSD=2.1%(n=9)。克罗米通在0.1006mgWmL～1.006mgWmL的浓度范围内线性关系良好,相关系数为0.9999,高、中、低浓度平均回收率为100.4%,RSD=0.93%(n=9)。结论:本方法结果准确可靠,可操作性强,可以更好的控制产品质量。
Objective:To develop a GC method for determination of ethanol and a HPLC method for assay for crotamiton to improve the current control method for Compound Diphenhydramine and Crotamiton Tincture and to control the product better.Methods:Determination of ethanol:a column packed with diethylene benzene-ethylethylene benzene porous polymer beads with the diameter of 0.25～0.18mm as the stationary phase was used,and maintain the column temperature at 190℃,a hydrogen flame ionization detector was used.Alternatively,a silica capillary column coated with 100% dimethylpolysiloxane as the stationary phase was used,and the column temperature was programmed:kept at 60℃ for 3minutes,and then increased by 20℃/min to 250℃.Samples were diluted with internal solution(0.2% propanol in N,N-dimethylformamide).Peak area was quantified by internal standard method.Assay for crotamiton:Venusil MP-C18 column was used.The column temperature was ambient.The mobile phase consisted of phosphate buffer(0.05mol/L potassium dihydrogen phosphate solution,consisting 1% triethylamine,adjust the pH value to 4.0)and acetonitrile(60:40,v/v),at a flow rate of 1.0ml/min.UV wavelength was 242nm;samples were diluted 10 times with ethanol and then diluted 10 times with the mobile phase and then filtered.Peak area was quantified by external standard method.Results:Determination of ethanol:the calibration curve was linear with the range of 0.3924mg/ml～5.886mg/ml,and correlation coefficient was 0.9999.The average recovery rate was 99.6% and the RSD was 2.1%(n=9).Assay for crotamiton:the calibration curve was linear with the range of 0.1006mg/ml～1.006 mg/ml,and correlation coefficient was 0.9999.The average recovery rate was 100.4% and the RSD was 0.93%(n=9).Conclusion:The methods are accurate,easy to operate and can control the product quality better.
出处
《中国药物应用与监测》
CAS
2006年第5期25-29,共5页
Chinese Journal of Drug Application and Monitoring
