摘要
目的:建立一种采用自身对照加校正因子法测定前列地尔尿道栓中前列腺素 A_1(PGA_1)及用自身对照法测定其它有关物质的方法。方法:以 Kromasil ODS 为分析柱(4.6mm×150mm,5μm,柱温30℃),以0.0067mol·L^(-1)磷酸二氢钾溶液-乙腈(57:43)为流动相,流速:1.0mL·min^(-1),检测波长为210nm。采用前列腺素 A_1(PGA_1)(美国药典 PGA_1对照品)的相对保留时间来确定 PGA_1的峰位置。用 PGA_1与前列腺素 E_1(PGE_1)对照品测定两者峰面积的比值,作为校正因子。结果:PGE_1和PGA_1分别在0.049～2.5mg·mL^(-1)、4.7～296μg·mL^(-1)浓度范围内与峰面积呈线性关系(r=0.9992、r=0.9998),PGE_1和PGA_1平均回收率分别为99.8%(PSI)为0.69%)、99.9%(PSD 为0.93%),样品溶液在7h 内稳定,PGA_1最低检测限为3.6ng,PGA_1与 PGE_1峰面积的相对保留时间在2.2～2.8之间(n=46),其平均值为2.5,校正因子为7.28(n=15)(RSD 为0.55%)。结论:方法简便、准确、可靠,适用于产品中已知杂质 PGA_1及其它有关物质的含量测定。
Objective：The self contrast and corrected factor method was established to determinate of Prostaglandihum A1 （ PGA1 ）, the self contrast method was used to determinate related substances of A1prostadil urethral suppository. Method：The column：Kromasil - C18 column（4. 6 mm mm×150mm,5μm,column temperature 30 ℃ ） ;The mobile phase ： 0. 0067 mol·L^-1potassium dihydrogen phosphate - acetonitrile （ 57 ： 43 ） ; The flow rate ： 1.0 mL ·min^-1 ;The detection wavelength：210 nm. PGA1 was determined by the relative retention time of PGA1 （American pharmacopoeia PGA1 reference standard）. Meanwhile, the corrected factor was the ratio value of the both peak areas of reference substances of PGA1 and PGEl. Result：The linear ranges for PGEl and PGA1were 0. 049 -2.5 mg ~ mL- 1 （ r = 0. 9992 ） and 4. 7 - 296 I.Lg ~ mL - 1 （ r = 0. 9998 ）, respectively. The average recovery rates （ n = 9 ） of PGEland PGA1were 99.8% （ RSD = 0. 69% ） and 99.9% （ RSD = 0. 93% ）, respectively. PGEland PGA1were steady in methanol within 7 hours. The measurable lowest limit of PGA1was 3.6 ng. Average value and range of the relative retention time of PGA1 peak and PGE1 peak were 2.48（n =46） and 2. 2 -2. 8. Corrected Factor was 7. 28 （ n = 15 ） （ RSD = 0. 55% ）. Cunclusion： This method is simple, accurate, reliable. It was suitable for the content determination of known impurity - PGA1 and related substance in the drug.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2006年第6期836-839,共4页
Chinese Journal of Pharmaceutical Analysis
