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目的:建立一种快速、准确、灵敏的高效液相色谱-质谱(HPLC-MS)法同时测定人血浆中米屈肼和左卡尼汀的浓度。方法:以卡巴胆碱作为内标,血浆样品经蛋白沉淀法处理,用氰基色谱柱(Ultimate XB-CN,4.6 mm×250 mm,5μm)进行分离,以乙腈-30 mmol·L~(-1)醋酸铵水溶液(含0.08%甲酸)(80:20,v/v)为流动相,流速1.0 mL·min~(-1),柱温40℃,柱后分流比为4:1,HPLC-MS/ESI~+法选择性监测准分子离子峰[M+H]~+(米屈肼m/z 147.1,左卡尼汀m/z 162.1,内标卡巴胆碱m/z147.1)。结果:米屈肼、左卡尼汀及内标卡巴胆碱在氰基柱上保留较好,分离完全;米屈肼、左卡尼汀线性范围分别为0.1～30.0μg·mL~(-1)(r=0.9985)和0.4～12.8μg·mL~(-1)(r=0.9994);最低定量限分别为0.1μg·mL~(-1)和0.4μg·mL~(-1);平均萃取回收率均大于80%,方法回收率为92%～114%;日内日间RSD均小于12%。结论:本方法简便准确,可用于同时测定人血浆中米屈肼和左卡尼汀的浓度,考察服用米屈肼对血浆中内源性物质左卡尼汀浓度的影响。
Objective: To establish a rapid, accurate and sensitive HPLC-MS method for the simultaneous determination of mitomycin and levocarnitine in human plasma. Methods: Carbachol was used as an internal standard. The plasma samples were separated and purified by protein precipitation, and separated on a Cyan column (Ultimate XB-CN, 4.6 mm × 250 mm, 5 μm) 1) ammonium acetate aqueous solution (containing 0.08% formic acid) (80:20, v / v) as mobile phase at a flow rate of 1.0 mL · min -1 .The column temperature was 40 ℃. (M + H] ~ + (Meldonium m / z 147.1, levocarnitine m / z 162.1, internal standard carbachol m / z 147.1) . Results: Meldonium, L-carnitine and internal standard carbachol retained well on the cyano-column and the separation was complete. The linear ranges of Meldonium and L-carnitine were 0.1 ~ 30.0μg · mL -1 ) (r = 0.9985) and 0.4 ~ 12.8μg · mL -1 (r = 0.9994) .The lowest limit of quantification was 0.1 μg · mL -1 and 0.4 μg · mL -1, respectively. The mean The recoveries of extraction were more than 80%, and the recoveries were 92% -114%. The intraday RSDs were less than 12%. Conclusion: The method is simple and accurate, and can be used to determine the concentration of Meldonium and L-Carnitine in human plasma at the same time. The effect of mometralhydrazine on the concentration of levocarnitine in plasma is investigated.