育发产品中斑蝥素和氮芥及米诺地尔的液相色谱-串联质谱测定法

Determination of cantharidin,nitrogen mustard and minoxidil in nurturing hair products by liquid chromatography-tandem mass spectrometry

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 develop a method of liquid chromatography-tandem mass spectrometry （LC-MS-MS） for the determination of eantharidin, nitrogen mustard and minoxidil in nurturing hair products. Methods The diluted samples were detected by multiple reaction monitoring（MRM） acquisition under positive ion mode with isocratic elution using 95% methanol （containing 0.2% ammonia） and 5% acetonitrile as mobile phases by Waters symmetry C18 column （4.6 mmx250 ram,5 pro1）. Results The linear ranges of cantharidin,nitrogen mustard and minoxidil were 5.00-500,5.00-1 000 and 0.100-50.0 ng/ml respectively. The regression equations showed a good linearity with the correlation coefficients more than 0.999. The limits of detection （LOD） for eantharidin, nitrogen mustard and minoxidil were 2.0,3.4 and 0.04 Ixg/g, the limits of quantification （LOQ） were 6.4,11.0 and 0.10 txg/g respectively. The spiked recoveries ranged from 94.5% to 104.7%. The relative standard deviations （RSD） were less than 9%. Conclusion The established method is sensitive and has good selectivity, and it is applicable to the simultaneous determination of cantharidin,nitrogen mustard and minoxidil in nurturing hair products.