高效液相色谱-质谱联用法测定风湿免疫病患者口服低浓度甲氨蝶呤的血药浓度

发布时间：2019-05-23 04:38

【摘要】：目的建立风湿免疫病患者服用甲氨蝶呤的液相色谱-质谱联用血药浓度测定方法。方法采用甲醇沉淀蛋白,以氨基蝶呤作为内标,用Epic C18色谱柱(4.6 mm×50 mm,3μm),甲醇(含0.1%甲酸)-水(含0.1%甲酸)为流动相,梯度洗脱,流速0.6 m L·min~(-1),柱温40℃。用电喷雾离子化源,正离子模式,多反应监测(MRM)扫描方式进行监测。考察方法的专属性、标准曲线、定量下限、精密度、准确度、回收率、基质效应和稳定性。结果甲氨蝶呤在0.5~200.0 ng·m L~(-1)范围内线性良好(r=0.999 2),定量下限为0.5ng·m L~(-1),日内、日间精密度及准确度RSD15%,回收率为76.80%~85.49%。结论该检测方法快速、灵敏,满足对服用甲氨蝶呤72 h内的风湿免疫病患者血药浓度的准确测定。
[Abstract]:Objective to establish a liquid chromatography-mass spectrometry (LC-MS) method for the determination of methotrexate in patients with rheumatic immune disease. Methods the protein was precipitated by methanol, aminopterin was used as internal standard, Epic C18 column (4.6 mm 脳 50 mm, 3 渭 m) was used, methanol (containing 0.1% formic acid)-water (containing 0.1% formic acid) was used as mobile phase, gradient eluting. The flow rate is 0.6 mL 路min ~ (- 1) and the column temperature is 40 鈩，

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