QuEChERS-液相色谱-串联质谱法同时测定洗发水中11种抗真菌药物  

Simultaneous determination of 11 antifungal drugs in shampoos by QuEChERS-liquid chromatography tandem mass spectrometry

作　　者：宋玉琴 董芳 张娟 SONG Yu-qin;DONG Fang;ZHANG Juan(Zibo Institute for Food and Drug Control,Zibo,Shandong 255086,China)

机构地区：[1]淄博市食品药品检验研究院,山东淄博255086

出　　处：《日用化学品科学》2021年第10期48-52,共5页Detergent & Cosmetics

摘　　要：建立了QuEChERS-液相色谱-串联质谱法同时测定洗发水中灰黄霉素、酮康唑、克霉唑、益康唑等11种抗真菌药物的检测方法。样品采用甲醇提取,PSA吸附剂净化;LC部分采用0.1%甲酸水溶液为流动相A,0.1%甲酸的甲醇溶液为流动相B,梯度洗脱,进样量为2μL,流速为0.4 mL/min,柱温为30℃;MS部分采用电喷雾离子源、正离子多反应监测模式(MRM)测定,标准曲线法定量。结果表明,11种抗真菌药物的线性范围为20~1000 ng/mL,相关系数大于0.99,检出限为0.001~0.20μg/g;在低、中、高3种加标质量浓度下,11种抗真菌药物的平均回收率为88.4%~111.2%,相对标准偏差(RSD,n=5)为0.9%~5.1%。该方法具有良好的选择性、灵敏度和准确性,可用于洗发水中11种非法添加抗真菌药物的同时测定。A QuEChERS-liquid chromatography(LC)-tandem mass spectrometry(MS)method for simultaneous determination of 11 antifungal drugs including griseofulvin,ketoconazole,clotrimazole,econazole,etc.in shampoos was established.The samples were extracted with methanol and purified with PSA adsorbent.In the LC part,0.1%aqueous solution of formic acid was used as the mobile phase A,and the solution of 0.1%formic acid in methanol was used as the mobile phase B;gradient elution was used;the injection volume was 2μL;the flow rate was 0.4 mL/min;the column temperature was 30℃.In the MS part,the sample was determined by using electrospray ion source and positive ion multiple reaction monitoring mode(MRM);the standard curve method was used for quantitative analysis.The results show that the linear range of 11 antifungal drugs is 20~1000 ng/mL;the correlation coefficient is larger than 0.99;the limit of detection is 0.001~0.20μg/g.The average recovery rate of the 11 antifungal drugs is 88.4%~111.2%at the low,medium and high spiked mass concentrations.The relative standard deviation(RSD,n=5)is in the range of 0.9%~5.1%.This method has good selectivity,sensitivity and accuracy,and can be used for simultaneous determination of the 11 illegally added antifungal drugs in shampoos.

关 键 词：液相色谱-串联质谱 QuEChERS法 洗发水 抗真菌药物 

分 类 号：TQ658[化学工程—精细化工]