摘要
目的建立人体血浆中左炔诺孕酮浓度测定的LC-MS-MS法。方法血浆中目标成分采用乙酸乙酯萃取。色谱柱为BDSHypersil C18柱（3μm，2．1mm×50mm），以水（含0．5‰甲酸）-乙腈-甲醇（18：32：50）为流动相，流速为0．20mL·min^-1，采用ESI^＋MRM方式进行离子监测。质谱检测条件：离子源电压5．0kV，加热毛细管温度：300℃，鞘气（N2）流速：20L·Min^-1，辅助气流速：2L·min^-1。结果血浆中左炔诺孕酮在0．313～40．0ng·mL^-1。线性关系良好（r=0．9993），最低定量限为0．313ng·mL^-1，方法回收率为91．0％～105．7％，萃取回收率为77．2％～80．8％，日内及日间RSD均〈15％。结论本方法灵敏、准确，适用于临床试验中生物样品定量分析。
Objective To develop an LC-MS-MS method for the determination of levonorgestrel in human plasma. Methods After ethyl acetate induced extraction from the plasma samples, levonorgestrel was suhiected to LC-MS-MS analysis using electro-spray ionization. The MS system was operated in the multiple reaction monitoring mode. Chromatographic separation was performed on a Hypersil BDS C18 column （3μm, 2.1 min×50 mm）. The MS detection parameters were as follows： the capillary voltage was 5 kV, capillary temperature was 300 ℃, sheath gas flow rate was 20 L · min^-1 , and AUX/sweep gas flow rate was 2 L · min^-1. Results The linear calibration curves were at 0. 313- 40. 0 ng · mL^-1 for levonorgestrel. The lower limit of quantification of the method was 0. 313 ng · mL^- 1 for levonorgestrel. The intra and inter-day precisions were less than 15%. The method recovery was 91.0 %-105.7 %, and the extraction recovery was 77.2%-80.8%. Conclusion The method is highly sensitive and selective, suitable for the analysis of levonorgestrel in human plasma.
出处
《中南药学》
CAS
2008年第6期666-669,共4页
Central South Pharmacy
