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建立了液相色谱-串联质谱法测定卡非佐米(1)中的吗啉乙酸(2)和基因毒性杂质,(2S)-2-氨基-4-甲基-1-[(2R)-2-甲基环氧乙烷基]-1-戊酮(3)。采用Waters Xbridge Shield RP18色谱柱,以1 mmol/L乙酸铵溶液(用乙酸调至p H 5.5)∶乙腈(30∶70)为流动相。质谱采用三重四极杆质谱检测器,正离子多反应监测模式(MRM),监测离子对m/z 146.1?m/z 100.1(2)和m/z 172.2?m/z 86.1(3)。2和3分别在100~3 000 ng/ml和10~300 ng/ml范围内线性关系良好;定量限(LOQ)为100和10 ng/ml。平均回收率为99.6%和99.7%,RSD为1.4%和1.3%。
A method for the determination of morpholine acetic acid (2) and genotoxic impurities in carbofzl (1) by liquid chromatography-tandem mass spectrometry was established. The activities of (2S) -2-amino- 2-methyloxiranyl] -1-pentanone (3). A Waters Xbridge Shield RP18 column was used with 1 mmol / L ammonium acetate solution (adjusted to pH 5.5 with acetic acid): acetonitrile (30:70) as the mobile phase. The mass spectra were monitored by triple quadrupole mass spectrometry with a positive ion multiple reaction monitoring mode (MRM) of 146.1 μm / z 100.1 (2) and m / z 172.2 μm / 86.1 (3). 2 and 3 showed good linearity in the range of 100-3000 ng / ml and 10-300 ng / ml, respectively. LOQs were 100 and 10 ng / ml, respectively. The average recovery was 99.6% and 99.7% with RSDs of 1.4% and 1.3%.