摘要
目的:建立胎盘植入产妇术后人乳中甲氨蝶呤含量测定的固相萃取-高效液相色谱法。方法:乳汁样品经C18固相萃取小柱提取后进样测定,色谱柱为Agilent ZOBAX SB-C18(4.6 mm×250 mm,5μm)柱,流动相为0.05%醋酸溶液-乙腈(88∶12),流速为1.0 mL.min-1,检测波长为306 nm。结果:乳汁中甲氨蝶呤在0.5~5μg.mL-1浓度范围内线性关系良好,高、中、低浓度的方法回收率分别为99.8%,100.9%,99.1%;RSD均小于10%。日内和日间精密度均小于5.8%。结论:本方法专属性强,灵敏度高,操作简便,适用于乳汁中甲氨蝶呤含量的测定。
Objective:To estabilish a solid phase extraction and high performance liquid chromatography(SPE-HPLC)method for determination of methotrexate in human milk of placenta implantation women.Methods:Milk samples were prepared with C18solid phase extraction column.The chromatographic separation was performed on a Agilent ZOBAX SB-C18(4.6 mm×250 mm,5 μm) column.The mobile phase consisted of 0.05% acetic acid-acetonitrile(88∶ 22),flow rate was 1.0 mL·min-1.The detection wavelength was 306 nm.Results:The linear range for methotrexate was 0.5-5 μg·mL-1.The average recoveries of high,middle and low three concentration were 99.8%,100.9% and 99.1%,RSD were both less than 10%.The intra-day and inter-day RSD were less than 5.8%.Conclusion:The method is accurate,sensitive and simple,and suitable for the determination of methotrexate concentration in human milk.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2011年第12期2305-2307,共3页
Chinese Journal of Pharmaceutical Analysis