高效液相色谱法测定屈螺酮炔雌醇片的有关物质  

Determination of related substances of drospirenone and ethinylestradiol tablets by HPLC

作　　者：李志芳[1] 赵雪梅[1] 

机构地区：[1]广州市药品检验所,广州510160

出　　处：《中南药学》2017年第7期971-974,共4页Central South Pharmacy

摘　　要：目的建立屈螺酮炔雌醇片有关物质的检查方法。方法采用高效液相色谱法,Prontosil ACEeps色谱柱和Chromolith RP 18色谱柱串联,流动相A为乙腈-甲醇-水(203∶150∶550),流动相B为乙腈-甲醇-水(595∶150∶50),流速0.35 mL·min^(-1),进行梯度洗脱。紫外检测器和荧光检测器串联使用,(1)紫外检测波长222 nm(0~60 min);(2)荧光检测在0~37 min和42~60 min,激发波长215 nm,发射波长315 nm;在37~42 min,激发波长215 nm,发射波长344 nm;进样量为20μL。结果屈螺酮、炔雌醇与各杂质能有效分离,进样量在线性范围与峰面积线性关系良好(r为0.9998~0.9999),屈螺酮和炔雌醇的检测限分别为0.137μg·mL^(-1)和0.035μg·mL^(-1)(紫外检测),Δ9,11-炔雌醇和炔雌醇的检测限分别为0.0034μg·mL^(-1)和0.0042μg·mL^(-1)(荧光检测)。结论建立的方法准确,灵敏度高,可用于检查屈螺酮炔雌醇片的有关物质。Objective To determine the content of related substances in drospirenone and ethinylestradiol tablets. Methods HPLC method was adopted. Prontosil ACE-eps column and Chromolith RP 18 column were used, acetonitrile-methanol-water （203 ： 150 ： 550） as mobile phase A, and acetonitrile-methanol-water （595 ： 150 ： 50） the mobile phase B （gradient elution）, the flow rate was 0.35 mL · min^ - 1. The determination was performed by UV detector （222 nm for 0 - 60 min） in series with FLD detector, with excitation wavelength and emission wavelength 215 nm and 315 nm for 0 - 37 min and 42 - 60 min, 215 nm and 344 nm for 37 - 42 min. The injection volume was 20 μL. Results Drospirenone （or ethinylestradiol） and its related substances were separated effectively, with a good linearity （r was 0.9998 - 0.9999）. The LOD of drospirenone and ethinylestradiol was 0.137 μg·mL^- 1 and 0.035μg·mL^- 1 （UV detection）, and the LOD of Δ9, 11-ethinyloestradiol and ethinylestradiol was 0.0034μg·mL^- 1 and 0.0042 μg·mL^- 1 （FLD detection）. Conclusion This method is accurate, sensitive and suitable for the determination of related substances in drospirenone and ethinylestradiol tablets.

关 键 词：高效液相色谱法 屈螺酮炔雌醇片 有关物质 

分 类 号：R927[医药卫生—药学]