摘要
建立了超高效液相色谱-串联质谱法对食品接触用纸和纸板中异噻唑啉酮类杀菌剂含量进行快速测定。样品用甲醇重复提取后,旋转蒸发浓缩,甲醇复溶,同时以回收率为指标,结合响应曲面分析优化前处参数。以流动注射方式优化5种异噻唑啉酮类化合物的质谱参数,以电喷雾离子源正离子模式电离,结合多反应监测模式进行测定。5种异噻唑啉酮类化合物在5.0~200μg·L^-1范围内标准曲线线性良好,相关系数r均大于0.9989,平均回收率为82.1%~95.2%,方法检出限为5.0~10.0μg·kg^-1,方法定量限为15.0~35.0μg·kg^-1,相对标准偏差RSDs为5.15%~6.49%。该方法简单高效、回收率高、灵敏度高和重现性好均能达到分析测定要求,可用于食品接触用纸和纸板中异噻唑啉酮类杀菌剂的测定。
A method for determination of isothiazolinone fungicides in food contact paper and cardboard by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.Samples were extracted by methanol repeatedly,then rotary evaporation was carried out to concentrate the samples,finally the samples were redissolved by methanol.The recovery rate was used as an indicator to optimize the pre-processing parameters with the response surface analysis.The mass spectrometry parameters of five isothiazolinone compounds were optimized by flow injection under positive mode of the electron spray ionization(ESI+),data of the analytes were obtained with mass spectrometric multiple reaction monitoring(MRM)mode.Five isothiazolinone compounds exhibited good linearity with correlation coefficient(r>0.9989)when the concentrations ranged from 5.0 to 200μg/L.The average recoveries of three spike levels were 82.1%~95.2%,while the limits of detection and the limits of quantitation were ranged 5.0~10.0μg·kg^-1 and 15.0~35.0μg·kg^-1,respectively.The relative standard deviations(RSDs)were ranged 5.15%~6.49%.This method is easy to operate,and its recovery,sensitivity and reproducibility could achieve the requirements of determination for isothiazolinone fungicides in food contact paper and cardboard.
作者
郑学殷
黄嘉乐
许志彬
李瑞玲
曾广丰
ZHENG Xue-yin;HUANG Jia-le;XU Zhi-bin;LI Rui-ling;ZENG Guang-feng(National Quality Testing Center for Processed Food(Guangdong),Guangzhou Inspection and Testing Certification Group Company,Guangzhou Guangdong 511447,China;SGS-CSTC Standards Technical Services Co.,Ltd.,Guangzhou Guangdong 510000,China;Guangdong Inspection and Quarantine Technology Center,Guangzhou Guangdong 510623,China)
出处
《当代化工》
CAS
2020年第6期1253-1256,1260,共5页
Contemporary Chemical Industry
基金
广东省食品质量与安全重点实验室,基于脂质组学和稳定同位素技术结合化学计量学鉴定肉类真假(项目编号:2019KF005)
关键词
超高效液相色谱-串联质谱
食品接触用纸和纸板
异噻唑啉酮
杀菌剂
响应曲面优化
Ultra performance liquid chromatography-tandem mass spectrometry
Food contact paper and cardboard
Isothiazolinone
Fungicide
Response surface methodology
作者简介
郑学殷(1984-),男,广东广州人,研究方向:食品理化检测。E-mail:378617191@qq.com
