摘要
目的 :建立了GC -FID法测定注射用倍美力和倍美力软膏含量方法 :样品通过硫酸酯酶水解得到游离雌激素 ,经 1%三甲基氯硅烷的双 (三甲基硅烷 )三氟乙酰胺硅烷化后 ,用RtxR- 2 2 5 (15m× 0 2 5mm× 0 2 5 μm)弹性石英毛细管色谱柱 ,以 3-甲氧基雌酮为内标 ,程序升温分离雌酮、马烯雌酮、 17α -二氢马烯雌酮、 17α -雌二醇、 17β -雌二醇、 17β-二氢马烯雌酮。结果 :3个主要成分雌酮、马烯雌酮、 17α -二氢马烯雌酮分别在 80~ 480 μg·mL-1(r=0 9994) ,40~ 2 80 μg·mL-1(r =0 9997) ,2 0~ 170 μg·mL-1(r=0 9995 )的浓度范围内呈良好线性关系。雌酮、马烯雌酮、 17α-二氢马烯雌酮平均回收率分别为 10 0 6 % ,RSD =1 2 0 % ;10 0 0 % ,RSD=0 98% ;10 0 2 % ,RSD =1 5 0 %。结论 :本法选择性高、重现性好、准确、快速和应用简便。
Objective:The method of the determination of 17α-dihydroequilin,equilin and estrone in premarin for injection and in premarin cream using GC-FID by trimethylsilylating was developed.Method:The conjugated estrogens were hydrolyzed by sulfatase enzyme to free estrogens,the free estrogens were silylated by bis(trimethylsilyl) trifluoroacetamide containing 1% trimethyl-chlorosilane in combination with 3-O-methylestrone as an internal standard,the trimethylsilyl derivaties were chromatographed.The gas chromatograph was equipped with a flame-ionization detector held at 205 ℃ for 10 min.and increased to 230 ℃ by 2 ℃ peramin,a 0 25 mm×15 m fused-silica capillary column bonded with a 0 25 μm layer of Rtx R-225 or OV-225.Results:17α-dihydroequilin,equilin,estrone,17α-estradiol,17β-estradiol and 17β-dihydroequilin were separated and determined.The standard curves for estrone,equilin and 17α-dihydroequilin are linear in the range of 80~280 μg·mL -1 ,40~280 μg·mL -1 ,20~170 μg·mL -1 respectively.The average recoveries of estrone,equilin,17α-dihydroequilin at different concentration were 100 6%,100 0%,100 2% respectively,their RSDs were 1 20%,0 98%,1 50%(n=8).Conclusion:The method is simple,rapid,reliable and correct.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2001年第1期18-21,共4页
Chinese Journal of Pharmaceutical Analysis
关键词
毛细管气相色谱法
倍美力注射液
倍美力软膏
结合态雌激素
capillary gas chromatography,conjugated estrogens,conjugated estrogens for injection,conjugated estrogens in premarin cream,trimethylsilylating