气质联用法同时测定皮革及其制品中7种限用异噻唑啉酮类抗菌剂

建立了1个同时测定皮革及其制品中7种限用异噻唑啉酮类抗菌剂的气质联用分析方法,该方法以甲醇为萃取溶剂,超声萃取皮革及其制品中的目标分析物,萃取液经固相萃取柱净化后进行气相色谱/质谱-选择离子监测法测定,外标法定量。在信噪比为3(S/N=3)的条件下,MBIT、BBIT、OI检出限均为0.05 mg/kg,MI、CMI、BIT、DCOI检出限均为0.10 mg/kg。在3个加标浓度水平下,方法平均加标回收率为80.21%~95.87%,相对标准偏差(RSD,n=9)为1.26%~4.85%。该方法简便快捷,定性可靠,定量准确,灵敏度高,检出限远低于相关法规限量要求,可完全满足皮革及其制品中限用异噻唑啉酮类抗菌剂日常检测的要求。

Simultaneous Determination of Seven Kinds of Restricted Isothiazolinone Antibacterial Agents in Leather and Leather Products by Gas Chromatography/Mass Spectrometry

An effective method was established for the simultaneous determination of seven kinds of restricted isothiazolinone antibacterial agents in leather and leather products using gas chromatography/mass spectrometry technique.The target compounds in leather and leather products were ultrasonically extracted using methanol as the extraction solvent.The extract was purified by solid phase extraction(SPE)column,followed by the analysis of gas chromatography/mass spectrometry in selected ion monitoring mode(GC/MS-SIM).The concentration of each restricted isothiazolinone antibacterial agents was calibrated by the external standard method.The limit of detection(LOD)was all 0.05mg/kg for MBIT,BBIT and OI while all 0.10mg/kg for MI,CMI,BIT and DCOI,respectively,at the ratio of signal to noise of three(S/N=3).The blank samples were spiked at three spiked levels and the spiked average recoveries changed from 80.21%to 95.87%while the relative standard deviation(RSD,n=9)changed from 1.26%to 4.85%.The proposed method was simple,rapid,accurate and sensitive.The limit of detection(LOD)was far less than the limited requirement of relevant regulations.The proposed method could meet completely the demand on the routine analysis of restricted isothiazolinone antibacterial agents in leather and leather products.