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

关键词:  QuECHERS  液相色谱-串联质谱法  抗感染药物  去屑类发用产品

Key words:  QuECHERS  HPLC-MS/MS  anti-infective drugs  anti-dandruff hair products

摘要:

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ZORBAX SB-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0.056~1.89 μg·g^-1，检出限为0.014~0.56 μg·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。

Abstract:

OBJECTIVE To establish a QuECHERS-liquid chromatography-tandem mass spectrometry method for simultaneous determination of 3 triazole antifungal drugs including itraconazole, voriconazole, posaconazole, and 5 nitroimidazoles 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.