Hamamoto Kouko, Mizuno Yasuharu, Kato Masaki, Yamagishi Norio, Furuhama Kazuhisa
National Veterinary Assay Laboratory, Ministry of Agriculture, Forestry and Fisheries, 1-15-1 Tokura, Kokubunji, Tokyo, Japan.
J Vet Med Sci. 2013 May 2;75(4):509-13. doi: 10.1292/jvms.12-0220. Epub 2012 Nov 13.
A quantitative assay method using LC/ESI-MS/MS for simultaneous determination of MCP in cattle plasma was developed and validated. Chromatographic separation was carried out using a multimode column (2 × 150 mm, 3 μm) with gradient elution (0.05% formic acid/methanol with 0.05% formic acid). MCP and levosulpiride (internal standard) were analyzed in the precursor/product ion pair of m/z 300.1/226.9 and 342.0/112.0, respectively. Linear calibration curves were obtained in the range of 2.5-500 ng/ml (R(2)>0.999) with a lower limit of quantification of 0.05 ng/ml. Mean recoveries were 96-103%, and the coefficient of variation was less than 6.5%. Plasma MCP concentrations after intravenous administration at 0.4 mg/kg to 12 cattle were determined by the LC-MS/MS method.
建立并验证了一种使用液相色谱/电喷雾串联质谱法同时测定牛血浆中MCP的定量分析方法。采用多模式柱（2×150 mm，3μm）进行梯度洗脱（0.05%甲酸/甲醇与0.05%甲酸）以实现色谱分离。分别在质荷比为300.1/226.9和342.0/112.0的前体/产物离子对中分析MCP和左舒必利（内标）。在2.5 - 500 ng/ml范围内获得线性校准曲线（R(2)>0.999），定量下限为0.05 ng/ml。平均回收率为96 - 103%，变异系数小于6.5%。采用液相色谱 - 串联质谱法测定了12头牛静脉注射0.4 mg/kg后血浆中的MCP浓度。
