高效液相色谱-串联质谱法测定化妆品中禁用磺胺和喹诺酮类化合物  

Simultaneous determination of sulfonamides and quinolones antibiotics in cosmetics by high-performance liquid chromatography-tandem mass spectrometry

作　　者：杨飘飘 张静雅 刘红 李丽霞 Piaopiao Yang;Jingya Zhang;Hong Liu;Lixia Li(Hubei Institute for Drug Control,Wuhan,Hubei 430075,China;Hubei Engineering Research Center for Drug Quality Control,Wuhan,Hubei 430075,China)

机构地区：[1]湖北省药品监督检验研究院,湖北武汉430075 [2]湖北省药品质量检测与控制工程技术研究中心,湖北武汉430075

出　　处：《日用化学工业（中英文）》2024年第8期997-1007,共11页China Surfactant Detergent & Cosmetics

基　　金：湖北省药品监督检验研究院中青年科研项目(2022YN005)。

摘　　要：建立了高效液相色谱-串联质谱法同时测定化妆品中喹诺酮类、磺胺类等53种抗感染药物的检测方法。样品采用饱和氯化钠分散,体积分数1%甲酸-乙腈溶液超声提取,离心后,以0.1%甲酸水溶液(含1 mmol/L乙酸铵)和0.1%甲酸-甲醇溶液作为流动相,梯度洗脱,并采用电喷雾离子源、正离子多反应监测模式(MRM)测定,外标法定量。结果表明,53种禁用原料线性拟合良好,相关系数大于0.9910,检出限为0.01~0.1μg/g,在低、中、高3种加标质量浓度下,磺胺类和喹诺酮类的平均回收率为80.84%~115.09%。筛查的100批次样品中有1批次样品检出磺胺甲噁唑。该方法具有良好灵敏度、选择性和准确性,可用于化妆品中53种抗感染药物测定。A method for simultaneous determination of 53 anti-infective drugs such as quinolones and sulfonamides in cosmetics was established by high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were dispersed with saturated sodium chloride,extracted by ultrasound with 1%acetonitrile formate solution,and centrifuged.0.1%Formic acid aqueous solution(containing 1 mmol/L ammonium acetate)and 0.1%formic acid methanol solution were chose as mobile phase,gradient elution was used,and electrospray ion source,positive ion multi-reaction monitoring mode(MRM)were used for determination with quantitative external standard method.The results show that the linear fitting of the 53 banned raw materials is good,with the correlation coefficient greater than 0.9910,and the detection limit of 0.01-0.1μg/g.The average recovery rates of sulfonamides and quinolones are 80.84%to 115.09%at low,medium,and high spiked mass concentrations.Among the 100 batches of samples screened,1 batch is detected to contain sulfamethoxazole.The method has good sensitivity,selectivity and accuracy,and can be used for the determination of 53 anti-infective drugs in cosmetics.

关 键 词：高效液相色谱-串联质谱法 磺胺类 喹诺酮类 

分 类 号：TQ658[化学工程—精细化工]