固相萃取－高效液相色谱法测定人乳中甲氨蝶呤的含量

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,5 μm)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0.5～5 μg·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.

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