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目的建立了育发产品中斑蝥素、氮芥和米诺地尔的液相色谱-串联质谱(LC-MS-MS)测定方法。方法样品经直接稀释1 000倍,以95%甲醇(含0.2%氨水)-5%乙腈为流动相进行等度洗脱,选用Waters symmetry C18(4.6 mm×250 mm,5μm)色谱柱,正离子模式下质谱多反应监测(MRM)模式检测。结果斑蝥素、氮芥和米诺地尔分别在5.00~500、5.00~1 000和0.100~50.0 ng/ml的范围内,所得的回归方程均呈较好的线性关系(r≥0.999),检出限分别为2.0、3.4、0.04μg/g定量下限分别为6.4、11.0、0.10μg/g,回收率在94.5%~104.7%之间,RSD<9%。结论该方法灵敏度高,选择性强,适用于育发产品中斑蝥素、氮芥和米诺地尔的测定。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS-MS) method for the determination of cantharidin, mechlorethamine and minoxidil in hair-growing products. Methods The samples were directly diluted 1 000 times with 95% methanol (containing 0.2% ammonia) -5% acetonitrile as mobile phase for isocratic elution. The sample was separated on a Waters symmetry C18 column (4.6 mm × 250 mm, 5 μm) Mode mass spectrometry multiple reaction monitoring (MRM) mode detection. Results The results showed that the regression equations of cantharidin, mechlorethamine and minoxidil were in the range of 5.00 ~ 500,5.00 ~ 1 000 and 0.100 ~ 50.0 ng / ml, respectively. The regression equation showed a good linear relationship (r≥0.999) The limits of quantification were 2.0, 3.4 and 0.04 μg / g, respectively, and the lower limits of quantitation were 6.4, 11 and 0.10 μg / g, respectively. The recoveries ranged from 94.5% to 104.7% with a RSD <9%. Conclusion The method is highly sensitive and selective and suitable for the determination of cantharidin, nitrogen mustard and minoxidil in hair products.