超高效液相色谱-串联质谱联用快速测定纺织品中多种双酚类化合物  

Rapid Determination of Multiple Bisphenol Compounds in Textiles by Ultra Performance Liquid Chromatography Coupled with Quadrupole Mass Spectrometry

作　　者：吴刚 吴冰婵 阮凯 王力君 来燕芳 王忠才 WU Gang;WU Bing-Chan;RUAN Kai;WANG Li-Jun;LAI Yan-Fang;WANG Zhong-Cai(Hangzhou Customs Technology Center,Hangzhou 311215;Hubei Province Ecological Environment Monitoring Center Station,Wuhan 430071;Zhejiang Academy of Science and Technology for Inspection&Quarantine,Hangzhou 311215)

机构地区：[1]杭州海关技术中心,杭州311215 [2]湖北省生态环境监测中心站,武汉430071 [3]浙江省检验检疫科学技术研究院,杭州311215

出　　处：《中国口岸科学技术》2025年第3期54-62,共9页China Port Science and Technology

基　　金：海关总署科研项目(2022HK121)。

摘　　要：本研究采用超高效液相色谱-串联质谱(Ultra Performance Liquid Chromatography Tandem Mass Spectrometry,UPLC-MS/MS)联用技术,建立了一种在5 min内快速分离和测定纺织品中12种双酚类化合物的方法。样品经甲醇超声提取,用孔径为0.22μm有机相针式过滤头过滤后,采用Acquity UPLC?BEH C18色谱柱(100 mm×2.1 mm i.d.,1.7μm)分离,以甲醇-水溶液为流动相进行梯度洗脱,目标分析物采用电喷雾(Electrospray Ionization,ESI)负离子多反应监测(Multiple Reaction Monitoring,MRM)模式进行测定,以保留时间和监测离子对进行定性定量分析。结果显示,该方法检出限(Limit of Detection,LOD)为0.02~0.08μg/kg,方法定量限(Limit of Quantitation,LOQ)为0.07~0.27μg/kg;在0.1~1.0μg/mL浓度范围内线性关系良好,添加浓度分别为0.5 mg/kg、1.0 mg/kg和5.0 mg/kg时,添加回收率范围为(82.45±6.81)%~(103.46±9.46)%,相对标准偏差为5.04%~11.51%。该方法选择性强、灵敏度高、操作简便、准确可靠,能够快速定性、定量地分析纺织品中多种双酚类化合物。A novel method has been developed to rapidly separate and determine 12 bisphenol compounds in textiles by ultra performance liquid chromatography-quadrupole mass spectrometry(UPLC-MS/MS)within 5 minutes.The bisphenol compounds in textiles were extracted by ultrasonic extraction with methanol,and then filtered through a 0.22μm organic phase needle filter head.The chromatographic analysis was performed by an Acquity UPLC?BEH C18 column(100 mm×2.1 mm i.d.,1.7μm)with a gradient elution of methanol and water as the mobile phase.The analytes were qualitatively and quantitatively detected by using electrospray ionization(ESI)tandem mass spectrometry with multiple reaction monitoring(MRM)in negative ion mode,based on retention times and monitoring ion pairs.The calibration curves showed good linearity in the range of 0.1-1.0μg/mL for all bisphenol compounds with the limits of determination(LOD)of 4-12μg/kg.The recoveries of 12 bisphenol compounds at the spiked concentration levels of 0.5,1.0 and 5.0 mg/kg ranged from 82.45±6.81%to103.46±9.46%with RSD of 5.04%-11.51%.This method is selective,highly sensitive,easy to operate,accurate,and reliable,providing a rapid and efficient approach for the qualitative and quantitative analysis of multiple bisphenol compounds in textiles.

关 键 词：超高效液相色谱-串联质谱 快速测定 双酚类化合物 纺织品 

分 类 号：TS107[轻工技术与工程—纺织工程]