液相色谱-串联质谱法测定食品接触橡胶密封垫圈中7种抗氧化剂  

Determination of 7 Antioxidants in Rubber Seal Gaskets for Food Contact by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：程畅 卢立新[1,2] 潘嘹 卢莉璟[1,2] 陈曦 CHENG Chang;LU Li-xin;PAN Liao;LU Li-jing;CHEN Xi(Department of Packaging Engineering,School of Mechanical Engineering,Jiangnan University,Wuxi 214122,China;Jiangsu Key Laboratory of Advanced Food Manufacturing Equipment Technology,Wuxi 214122,China)

机构地区：[1]江南大学机械工程学院包装工程系,江苏无锡214122 [2]江苏省食品先进制造装备技术重点实验室,江苏无锡214122

出　　处：《分析测试学报》2021年第7期1074-1079,共6页Journal of Instrumental Analysis

基　　金：国家重点研发计划项目(2018YFC1603200,2018YFC1603202)。

摘　　要：采用液相色谱-串联质谱技术建立了食品接触橡胶密封垫圈中7种抗氧化剂(抗氧化剂ZKF、抗氧化剂259、抗氧化剂1035、抗氧化剂425、抗氧化剂2246、抗氧化剂1520、抗氧化剂565)的同时检测方法。样品经甲醇微波提取,Acquity UPLC BEH C_(18)(100 mm×2.1 mm,1.7μm)色谱柱分离,以乙腈-乙酸铵水溶液(5 mmol/L)为流动相进行梯度洗脱,在正、负离子模式下测定。结果显示,7种抗氧化剂在0.01~0.5 mg/L质量浓度范围内线性良好,相关系数(r^(2))均大于0.999。方法检出限(MLOD)为0.005~0.125 mg/kg,方法定量下限(MLOQ)为0.02~0.40 mg/kg,平均加标回收率为73.1%~120%,相对标准偏差(RSD,n=6)为0.70%~9.3%。该方法前处理简单,15 min内可同时完成7种抗氧化剂的检测,且检出限较低,可满足食品接触橡胶材料及制品中抗氧化剂的检测需要。A method was developed for the determination of residues of 7 antioxidants,i.e.antioxidant ZKF,antioxidant 259,antioxidant 1035,antioxidant 425,antioxidant 2246,antioxidant 1520 and antioxidant 565 in rubber seal gaskets for food contact by liquid chromatography-tandem mass spectrometry.By optimizing the chromatographic column,elution procedure and mass spectrometry conditions,the optimal detection conditions were determined.The rubber powder sample was obtained by freezing and grinding the rubber sample with a freezing grinding instrument.After comparing the recoveries of three kinds of filter membranes and high-speed centrifugation,the highspeed centrifugation method was adopted to pretreat the extract.In addition,three extraction methods including ultrasonic,reflux and microwave,and two extraction solvents including methanol and acetone were used to extract the antioxidants from the positive rubber powder samples to obtain the extraction solution.Microwave extraction with methanol was determined as the optimal pretreatment method with the extraction recovery and extraction efficiency as the evaluation indexes.The rubber powder samples(g)and methanol(mL)were mixed by the ratio of 1:20,then extracted at 50℃for 15 minutes under microwave condition.After high-speed centrifugation treatment,the extracted liquid samples were detected by liquid chromatography-tandem mass spectrometry.The separation was performed on an Acquity UPLC BEH C18(100 mm×2.1 mm,1.7μm)column by gradient elution with acetonitrile-ammonium acetate aqueous solution(5 mmol/L)as the mobile phase,and the determination was carried out in positive and negative ion modes.Results showed that the limits of detection(LOD),limits of quantitation(LOQ),method limits of detection(MLOD)and method limits of quantitation(MLOQ)for the 7 antioxidants were in the ranges of 0.003-0.083μg/L,0.01-0.25μg/L,0.005-0.125 mg/kg and 0.02-0.40 mg/kg,respectively.There were good linear relationships for the 7 antioxidants in the mass concentration range of 0.01-0.5 mg/L

关 键 词：液相色谱-串联质谱 食品接触橡胶密封垫圈 抗氧化剂 微波萃取 

分 类 号：O657.7[理学—分析化学] TS206.4[理学—化学]