皮革及其制品中7种限用异噻唑啉酮类抗菌剂的气相色谱/串联质谱法测定

建立了1个气相色谱/串联质谱分析方法,对皮革及其制品中7种限用异噻唑啉酮类抗菌剂进行同时测定。首先采用超声萃取技术提取皮革及其制品中残留的限用异噻唑啉酮类抗菌剂,提取物用Supelclean LC-Ph固相萃取柱进行净化处理后,进行气相色谱/串联质谱法分析,采用外标法对提取物进行定量。该方法灵敏度高,在10信噪比(S/N=10)条件下,BBIT、OI、MBIT的定量下限均为0.05 mg/kg,BIT、CMI、DCOI、MI的定量下限均为0.10 mg/kg,远低于相关法规的限量要求。采用空白加标测试方法来确定方法的回收率和精密度,在3个加标浓度水平下,加标平均回收率变化范围为80.25%~95.86%,相对标准偏差(RSD,n=9)变化范围为2.84%~12.75%。该方法简单快速、灵敏度高,可用于皮革及其制品中限用异噻唑啉酮类抗菌剂的日常测试。

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

An effective method was established to simultaneously determine seven kinds of restricted isothiazolinone antibacterial agents in leather and its products by gas chromatography/tandem mass spectrometry(GC/MS-MS)technique.Ultrasonic extraction technology was first used to extract the residual restricted isothiazolinone antibacterial agents in leather and its products,the extract was then purified with Supelclean LC-Ph solid phase extraction(SPE)column,gas chromatography/tandem mass spectrometry(GC/MS-MS)analysis was finally performed to determine the content of restricted isothiazolinone antibacterial agents.The concentration of each isothiazolinone antibacterial agents were calibrated by the external standard method.The proposed method had high sensitivity.Under the condition of 10 signal-to-noise ratio(S/N=10),the limit of quantification(LOQ)was all 0.05 mg/kg for BBIT,OI and MBIT and all 0.10 mg/kg for BIT,CMI,DCOI,and MI,respectively,far less than the limit requirements of relevant laws and regulations.The spiked blank test method was performed to determine the recovery and precision of the proposed method.The blank samples were spiked at three different concentration levels,the spiked average recovery varied in the range from 80.25%to 95.86%while the relative standard deviation(RSD,n=9)varied in the range from 2.84%to 12.75%.The proposed method was simple,rapid,and sensitive,and could be applied in the routine analysis of restricted isothiazolinone antibacterial agents in leather and its products.