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建立了采用超高效液相色谱-串联质谱测定兔血浆中丝裂霉素C的方法。以兔空白血浆为基质,通过添加标准溶液的方法配制含丝裂霉素C和内标物曲安奈德的样品,选用乙酸乙酯为提取溶剂,液-液萃取法处理血浆样品。采用Hypersil Gold C18分析柱(50 mm×2.1 mm,1.9μm),流动相为甲醇-0.1%甲酸水溶液(90∶10,v/v),等度洗脱,流速0.2 mL/min,柱温35℃,在3 min内实现了快速分离。采用电喷雾正离子(ESI+)模式电离,选择反应监测(SRM)模式检测,以曲安奈德作为内标物进行定量。用于监测的定量离子对分别为丝裂霉素C m/z 335.2→242.2和曲安奈德m/z 435.2→397.3/415.2,用基质匹配标准溶液法进行定量。结果表明:兔血浆中丝裂霉素C的质量浓度在1～1 000μg/L范围内线性关系良好(r=0.997 8,权重系数(weighting):1/x2);血浆中丝裂霉素C的检出限(信噪比为3)为0.2μg/L;其平均回收率为85%～115%;日内及日间的相对标准偏差(RSDs)均小于15%,满足生物样品检测的要求。该方法可用于兔气管外壁给药后的血浆样品中丝裂霉素C的检测。本方法选择性强、灵敏度高、操作简便快速、重现性好,适用于丝裂霉素C药代动力学等方面的研究。
A method for the determination of mitomycin C in rabbit plasma by ultra performance liquid chromatography-tandem mass spectrometry was established. Rabbit blank plasma was used as matrix to prepare mitomycin C and triamcinolone acetonide internal standard by adding standard solution. Ethyl acetate was used as extraction solvent and plasma-liquid extraction was used to treat plasma samples. Hypersil Gold C18 column (50 mm × 2.1 mm, 1.9 μm) was used. The mobile phase consisted of methanol-0.1% formic acid aqueous solution (90:10, v / v) with isocratic elution at a flow rate of 0.2 mL / ℃, in 3 min to achieve a rapid separation. Electrospray ionization (ESI +) mode ionization, selective reaction monitoring (SRM) mode detection and triamcinolone acetonide as internal standard were used. Quantitative ion pairs for monitoring were mitomycin C m / z 335.2 → 242.2 and triamcinolone acetonide m / z 435.2 → 397.3 / 415.2, respectively, and quantified using a matrix matching standard solution method. The results showed that the linearity of mitomycin C in rabbit plasma was linear in the range of 1 ~ 1000μg / L (r = 0.997 8, weighting: 1 / x2) The detection limit (signal to noise ratio of 3) was 0.2μg / L; the average recovery was 85% ~ 115%; the relative standard deviations (RSDs) were less than 15% . The method can be used for the detection of mitomycin C in plasma samples after administration of rabbit tracheal outer wall. The method has the advantages of strong selectivity, high sensitivity, simple and quick operation, good reproducibility and application in the research of mitomycin C pharmacokinetics and the like.