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目的:为了提高控制复方樟脑乳膏的质量,建立同时测定复方樟脑乳膏中樟脑、薄荷脑、水杨酸甲酯、苯海拉明4个主要成分含量的气相色谱方法。方法:采用聚乙二醇20M(DB-Wax)毛细管色谱柱(30 m×0.32 mm×1.80μm),氮气为载气,FID检测器,程序升温(初始温度120℃,维持8 min,升温速度50℃·min-1,最终温度240℃,维持12 min),萘为内标。结果:复方樟脑乳膏中樟脑、薄荷脑、水杨酸甲酯、苯海拉明、内标物萘以及各辅料获得良好分离,方法专属性强,线性范围宽,精密度好,准确度高,耐用性好。樟脑、薄荷脑、水杨酸甲酯、苯海拉明浓度分别在0.6464~16.16 mg·mL-1(r=0.9999)、0.4758~11.90 mg·mL-1(r=0.9999)、0.3360~8.400 mg·mL-1(r=0.9999)和0.1669~4.172 mg·mL-1(r=0.9999)范围内具有良好的线性关系,低、中、高浓度平均回收率(n=3)樟脑为99.3%(RSD=0.6%)、100.3%(RSD=0.6%)、100.0%(RSD=0.6%),薄荷脑为98.9%(RSD=0.4%)、100.0%(RSD=0.3%)、100.0%(RSD=0.6%),水杨酸甲酯为99.5%(RSD=0.4%)、99.7%(RSD=0.4%)、99.6%(RSD=0.8%),苯海拉明为99.4%(RSD=0.2%)、99.3%(RSD=0.6%)、99.5%(RSD=0.7%)。结论:该方法符合方法学验证要求,可用于控制复方樟脑乳膏的质量。建议国家药品标准提高修订复方樟脑乳膏含量测定控制方法并拟定限度。
OBJECTIVE: To establish a gas chromatographic method for the simultaneous determination of four main components of camphor, menthol, methyl salicylate and diphenhydramine in compound camphor cream by controlling the quality of compound camphor cream. Methods: Polyethylene glycol 20M (DB-Wax) capillary column (30 m × 0.32 mm × 1.80 μm) was used with nitrogen as the carrier gas and FID detector. The temperature was programmed (initial temperature was 120 ℃, maintained for 8 min, 50 ℃ · min-1, the final temperature of 240 ℃, maintaining 12 min), naphthalene as an internal standard. Results: Camphor, menthol, methyl salicylate, diphenhydramine, internal standard naphthalene and their excipients were well separated in the compound camphor cream, and the method was specific, linear, broad and precise, with high accuracy Good durability. The concentrations of camphor, menthol, methyl salicylate and diphenhydramine ranged from 0.6464 to 16.16 mg · mL -1 (r = 0.9999), 0.4758-11.90 mg · mL -1 (r = 0.9999), 0.3360-8.400 mg (R = 0.9999) and 0.1669 ~ 4.172 mg · mL-1 (r = 0.9999). The average recoveries of low, medium and high concentration (n = 3) were 99.3% for camphor 100.0% (RSD = 0.3%), 100.0% (RSD = 0.6%), 100.0% (RSD = (RSD = 0.4%), 99.6% (RSD = 0.8%), diphenhydramine 99.4% (RSD = 0.2%), methyl salicylate 99.5% , 99.3% (RSD = 0.6%), 99.5% (RSD = 0.7%). Conclusion: This method meets the validation requirements of methodology and can be used to control the quality of compound camphor cream. It is suggested that the national drug standards should be improved to revise the control method of compound camphor cream and to draw up limits.