QuECHERS-液相色谱-串联质谱同时测定去屑类发用产品中8种抗感染药物

Simultaneous Determination of 8 Anti-infective Drugs in Anti-dandruff Hair Products by QuEChERS-liquid Chromatography Tandem Mass Spectrometry

目的 建立QuECHERS-液相色谱-串联质谱法同时检测去屑类发用产品中3种三唑类抗真菌药(伊曲康唑、伏立康唑、泊沙康唑)和5种硝基咪唑类药物(洛硝哒唑、二甲硝咪唑、塞克硝唑、替硝唑、奥硝唑)的方法。方法 样品加入1 mL饱和氯化钠溶液并用乙腈提取,通过QuEChERS净化后过滤膜上机检测,以ZORBAXSB-C18色谱柱分离,0.1%甲酸乙腈-0.1%甲酸水溶液作为流动相梯度洗脱,电喷雾正离子模式(ESI+),多重反应监测扫描,基质外标法定量。结果 8种抗感染药物在20.0~1 000.0 ng·mL^(–1)内与峰面积均呈良好线性关系,相关系数均>0.995,在3个不同浓度添加水平下,平均加样回收率为90.3%~113.0%,相对标准偏差RSD(n=6)为0.4%~2.6%。方法的定量限为0.056~1.89μg·g^(–1),检出限为0.014~0.56μg·g^(–1)。结论 该方法具有快速简便,净化效果好的特点,可用于去屑类发用产品中8种抗感染药物的检测。

OBJECTIVE To establish a QuECHERS-liquid chromatography-tandem mass spectrometry method for simultaneous determination of 3 triazole antifungal drugs including itraconazole,voriconazole,posaconazole,and 5nitroimidazoles including ronidazole,dimetridazole,secnidazole,tinidazole and ornidazole.METHODS The sample was added into 1 mL of saturated sodium chloride solution and extracted with acetonitrile,and then purified by QuECHERS method.The separation was performed on a ZORBAX SB-C18 column.The mobile phase consisted of 0.1% formic acid acetonitrile-0.1%formic acid aqueous solution by gradient elution,electrospray ionization(ESI+) source was applied and operated in the positive mode.Multiple reaction monitoring mode was used to monitor ions.Matrix-matched calibration was used to quantitative calculation.RESULTS Eight anti-infective drugs showed good linear relationship in the range of 20.0-1 000.0 ng·mL^(-1).The linear correlation coefficients of the method were >0.995.At three levels,the average recoveries ranged from 90.3% to 113.0%,with the RSD(n=6) from 0.4% to 2.6%.The limits of quantification of the method were among 0.056-1.89 μg·g^(-1),and the limits of detection were among 0.014-0.56 μg·g^(-1).CONCLUSION This method is rapid,accurate and has good purification effect,which can be applied to the detection of 8 anti-infective drugs in anti-dandruff hair products.