高效液相色谱-串联质谱法同时测定染整助剂中5种异噻唑啉酮

Simultaneous determination of 5 isothiazolinones in auxiliaries by high performance liquidchromatography-tandem mass spectrometry

建立了高效液相色谱-串联质谱法同时测定染整助剂中5种异噻唑啉酮的分析方法。样品经甲醇超声波提取,Eclipse C_(18)柱(2.1 mm×100 mm,3.5μm)分离后,进行高效液相色谱-串联四极杆质谱外标法测定,流动相为甲醇-水。结果表明:该方法对MI、CMI、BIT的检出限和定量限分别为0.75 mg/kg和2.5 mg/kg,OI、DCOI的检出限和定量限分别为0.15 mg/kg和0.50 mg/kg;加标平均回收率为79.63%~108.78%,相对标准偏差为1.46%~8.24%;MI、CMI、BIT在0.05~0.50 mg/L,OI、DCOI在0.01~0.20 mg/L范围内线性相关系数大于0.99。该方法灵敏度高、重现性好,可满足染整助剂中异噻唑啉酮的检测要求。

A method for the simultaneous determination of isothiazolinones in dyeing and finishing auxiliaries is developed by using ultrasonic extraction and high performance liquid chromatography-tandem mass spec-trometry(HPLC-MS/MS).The sample is extracted using methanol.Eclipse C_(18) column(2.1 mm×100 mm,3.5μm)is used for chromatographic separation.The mobile phases are methanol and water.External standard method is used for quantitation.For dyeing and finishing auxiliaries samples,the detection limits of the method are 0.75 mg/kg for MI,CMI,BIT and 0.15 mg/kg for OI,DCOI.The quantitation limits of the method are 2.5 mg/kg for MI,CMI,BIT and 0.5 mg/kg for OI,DCOI.The recoveries are 79.63%-108.78%.The relative standard de-viations(RSDs)are 1.46%-8.24%.The correlation coefficient is more than 0.99 at the concentration range of 0.05-0.50 mg/L for MI,CMI,BIT,and 0.01-0.20 mg/L for 01,DCOl,showing good linearity.This method shows high sensitivity and good reproducibility,which is suitable for qualitative and quantitative determination of isothi-azolinones in dyeing and finishing auxiliaries.