Determination of Mifepristone in Human Plasma by High Performance Liquid Chromatography
摘 要
建立了测定血浆中米非司酮浓度的高效液相色谱分析方法.血浆样品以乙醚提取,常温下负压挥发至干,所得残渣用甲醇浸溶后进行测定.Spherisorb C18(250 mm×4.6 mm i.d.,5 μm)为色谱柱,流动相为甲醇-乙腈-水(50+25+25)溶液,检测波长为302 nm,用外标法定量.结果表明,在0.05~10.00 mg·L-1范围内呈线性,检出限为0.01 mg·L-1;平均回收率为98.2%,日内、日间平均精密度分别为7.0%,8.3%.米非司酮血浆样品的萃后残渣于-20 ℃可保存至少7d.
Abstract
An method for the determination of mifepristone in human plasma by high performance liquid chromatography was developed and validated. The plasma sample was extracted with ether which was removed by evaporation at room temperature under reduced pressure. The residue was taken up with methanol and the solution obtained was submitted to analysis by RP-HPLC. The chromatographic column of spherisorb C18 (250 mm×4.6 mm,i.d. 5 μm) was used in the analysis,and a solution containing methanol,acetonitrile and water mixed in the proportion of 50 to 25 to 25 was used as the mobile phase,passing through the column. Volume of the volumetric loop used was 20 μL. Ultra violet spectrophotometric detection was made at the wavelength of 302 nm with determination by the external standard method. Mifepristone was well separated in the HPLC,thus leading to high selectivity of determination. Linear relationship between the absorbance and concentration of mifepristone was obtained in the range of 0.05 to 10.00 mg·L-1 with a detection limit of 0.01 mg·L-1. Value of average recovery obtained by the recovery test was 98.2%. Precision test was made at 3 different concentration levels,average values of RSD′s (n=5) of within day test and between-day test obtained were 7.0% and 8.3% respectively. Residue of the sample obtained after extraction with ether and removal of ether by evaporation was proved to be stable for at least 7 days when preserved at -20 ℃ in the dry state.
中图分类号 O657.7
所属栏目 工作简报
基金项目 浙江省科技厅科技攻关项目(2006C33065)、安徽省人口和计划生育委员会专项基金、安徽省教育厅自然科学基金(2005KJ251)资助
收稿日期 2006/2/16
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备注郭智勇(1973-),男,江苏江都人,讲师,博士,从事色谱分析和电化学分析研究.
引用该论文: GUO Zhi-yong,WEI Dan-yi,CHU Cheng-ding,Yin Geng-xin,HE Ming-li,WU Jian-li,FU Ke-qin. Determination of Mifepristone in Human Plasma by High Performance Liquid Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2007, 43(1): 15~17
郭智勇,魏丹毅,储成顶,尹耕心,贺明莉,吴建力,傅克勤. 高效液相色谱法测定血浆中米非司酮[J]. 理化检验-化学分册, 2007, 43(1): 15~17
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参考文献
【1】Baulieu E E,Segal S J. The antiprogestin steroid RU 486 and human fertility control[M]. New York: Plenum Press,1985:1.
【2】Heikinheimo O,Kekkonen R,Lhteenmki P. The pharmacokinetics of mifepristone in humans reveal insights into differential mechanisms of antiprogestin action[J]. Contraception,2003,68(6):421-426.
【3】Leminen R,Ranta S,Von Hertzen H,et al. Pharmacokinetics of 10 mg of mifepristone[J]. Contraception,2003,68(6):427-429.
【4】Kekkonen R,Heikinheimo O,Mandelin E,et al. Pharmacokinetics of mifepristone after low oral doses[J]. Contraception,1996,54(4):229-234.
【5】Wang J,Shi W,Zhang G,et al. Tissue and serum levels of steroid hormones and RU 486 after administration of mifepristone[J]. Contraception,1994,49(3):245-253.
【6】Baulieu E E,Segal S J. The antiprogestin steroid RU 486 and human fertility control[M]. New York: Plenum Press,1985:99.
【7】Kawai S,Nieman L,Brandon D,et al. Pharmacokinetic properties of the antiglucocorticoid and antiprogesterone steroid RU 486 in man[J]. J Pharmacol Exp Ther,1987,241(2):401-406.
【8】F ldesi I,Falkay G,Kovács L. Determination of RU486 (mifepristone) in blood by radioreceptorassay;a pharmacokinetic study[J]. Contraception,1996,54(1):27-32.
【9】Heikinheimo O,Tevilin M,Shoupe D,et al. Quantitation of RU486 in human plasma by HPLC and RIA after column chromatography[J]. Contraception,1986,34(6):613-624.
【10】Changhai H,Yongen S,Zhihou Y,et al. Pharmacokinetic study of orally administered RU 486 in non-pregnant women[J]. Contraception,1989,40(4):449-460.
【11】Stith C,Hussian M D. Determination of mifepristone levels in wild canid serum using liquid chromatography[J]. J Chromatogr B,2003,794(1):9-15.
【12】中华人民共和国卫生部药典委员会.中国药典[M].北京:化学工业出版社,2000:193.
【2】Heikinheimo O,Kekkonen R,Lhteenmki P. The pharmacokinetics of mifepristone in humans reveal insights into differential mechanisms of antiprogestin action[J]. Contraception,2003,68(6):421-426.
【3】Leminen R,Ranta S,Von Hertzen H,et al. Pharmacokinetics of 10 mg of mifepristone[J]. Contraception,2003,68(6):427-429.
【4】Kekkonen R,Heikinheimo O,Mandelin E,et al. Pharmacokinetics of mifepristone after low oral doses[J]. Contraception,1996,54(4):229-234.
【5】Wang J,Shi W,Zhang G,et al. Tissue and serum levels of steroid hormones and RU 486 after administration of mifepristone[J]. Contraception,1994,49(3):245-253.
【6】Baulieu E E,Segal S J. The antiprogestin steroid RU 486 and human fertility control[M]. New York: Plenum Press,1985:99.
【7】Kawai S,Nieman L,Brandon D,et al. Pharmacokinetic properties of the antiglucocorticoid and antiprogesterone steroid RU 486 in man[J]. J Pharmacol Exp Ther,1987,241(2):401-406.
【8】F ldesi I,Falkay G,Kovács L. Determination of RU486 (mifepristone) in blood by radioreceptorassay;a pharmacokinetic study[J]. Contraception,1996,54(1):27-32.
【9】Heikinheimo O,Tevilin M,Shoupe D,et al. Quantitation of RU486 in human plasma by HPLC and RIA after column chromatography[J]. Contraception,1986,34(6):613-624.
【10】Changhai H,Yongen S,Zhihou Y,et al. Pharmacokinetic study of orally administered RU 486 in non-pregnant women[J]. Contraception,1989,40(4):449-460.
【11】Stith C,Hussian M D. Determination of mifepristone levels in wild canid serum using liquid chromatography[J]. J Chromatogr B,2003,794(1):9-15.
【12】中华人民共和国卫生部药典委员会.中国药典[M].北京:化学工业出版社,2000:193.
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