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目的:建立可同时检测育发液中斑蝥素、米诺地尔、雌三醇、雌二醇、睾酮、甲睾酮、雌酮、己烯雌酚、黄体酮9种禁限用物质的液相色谱-质谱法。方法:采用CAPCELL PAK MG C_(18)色谱柱(150 mm×2 mm,5μm)进行分离,以10 mmol·L~(-1)醋酸铵溶液(A)-乙腈(B)为流动相进行梯度洗脱(0~12 min,90%A→50%A;12~13 min,50%A→60%A;13~20 min,60%A;20~30 min,60%A→20%A;30~31 min,20%A→90%A;31~40 min,90%A),流速0.2 m L·min~(-1);使用加热电喷雾离子源,正负离子检测,采用选择反应监测扫描方式。结果:斑蝥素、米诺地尔、雌三醇、雌二醇、睾酮、甲睾酮、雌酮、己烯雌酚、黄体酮质量浓度分别在1~100、0.001~0.05、0.25~25、15~300、0.05~5、0.1~5、0.06~3、0.02~2、0.05~5μg·m L~(-1)范围内均有良好的线性关系(r≥0.998);最低检出浓度分别为1.25、0.001、0.25、15、0.05、0.1、0.08、0.02、0.05μg·g~(-1),最低定量浓度分别为5、0.005、1.25、75、0.25、0.5、0.3、0.1、0.25μg·g~(-1)。在12批育发液样品中检出2批非法添加了米诺地尔。结论:本研究建立的方法可同时定性定量检测育发液中性激素、斑蝥素与米诺地尔等9种禁限用物质。
OBJECTIVE: To establish a liquid chromatography-mass spectrometry (LC-MS / MS) method for the simultaneous determination of 9 restricted substances such as cantharidin, minoxidil, estriol, estradiol, testosterone, methyltestosterone, estrone, diethylstilbestrol and progesterone law. Methods: The separation was performed on a CAPCELL PAK MG C 18 column (150 mm × 2 mm, 5 μm). The gradient was performed with 10 mmol·L -1 ammonium acetate solution (A) -acetonitrile (B) Elution (0-12 min, 90% A → 50% A; 12-13 min, 50% A → 60% A; 13-20 min, 60% A; 20-30 min, 60% A → 20% A ; 30 ~ 31 min, 20% A → 90% A; 31 ~ 40 min, 90% A) at a flow rate of 0.2 m L · min -1; using heated electrospray ionization, positive and negative ion detection, Monitoring scan mode. Results: The concentrations of cantharidin, minoxidil, estriol, estradiol, testosterone, methyltestosterone, estrone, diethylstilbestrol and progesterone were 1 ~ 100,0.001 ~ 0.05,0.25 ~ 25,15 ~ 300, 0.05 ~ 5,0.1 ~ 5,0.06 ~ 3,0.02 ~ 2,0.05 ~ 5μg · m L ~ (-1), there was a good linear relationship (r≥0.998); the lowest detected concentrations were 1.25,0.001 , 0.25,15,0.05,0.1,0.08,0.02,0.05μg · g -1, the lowest concentration were 5,0.005,1.25,75,0.25,0.5,0.3,0.1,0.25μg · g ~ ( -1). Two batches of illogne added illegally were found in 12 batches of hairbrush samples. Conclusion: The method established in this study can simultaneously qualitatively and quantitatively detect 9 kinds of restricted substances such as neutral hormone, cantharidin and minoxidil in hair growth hormone.