超高效液相色谱-串联质谱法测定热凝固蛋制品中7种对羟基苯甲酸酯类防腐剂  

Determination of 7 kinds of parabens preservatives in hot coagulated egg products by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：宁晓盼 马晶晶 刘宇 王梦茹 滕颖 楼芸 殷耀 柳菡 张晓燕 丁涛 NING Xiao-Pan;MA Jing-Jing;LIU Yu;WANG Meng-Ru;TENG Ying;LOU Yun;YIN Yao;LIU Han;ZHANG Xiao-Yan;DING Tao(Animal,Plant and Food Inspection Center,Nanjing Customs,Nanjing 210019,China)

机构地区：[1]南京海关动植物与食品检测中心,南京210019

出　　处：《食品安全质量检测学报》2024年第21期32-40,共9页Journal of Food Safety and Quality

基　　金：海关总署科研项目(2021HK192、2021HK193)。

摘　　要：目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定热凝固蛋制品中对羟基苯甲酸酯类(parabens,PBs)防腐剂的定量分析方法。方法选取蛋黄酪、松花蛋肠2种样品做研究对象,样品经氢氧化钠水解后用甲醇、20%甲醇水溶液提取、离心,使用MAX固相萃取小柱净化、富集。使用Kinetex C18色谱柱(100 mm×4.6 mm,2.6μm)分离,以乙腈-5 mmol/L乙酸铵溶液为流动相,梯度洗脱,流速0.8 mL/min,在电喷雾离子源负离子(electron spray ionization,ESI-)模式和多反应监测(multi reaction monitoring,MRM)模式下监测,外标法定量。结果7种PBs在10.0~200.0 ng/mL线性范围内,相关系数均大于等于0.9990,检出限(limits of detection,LODs)为0.6μg/kg,定量限(limits of quantitation,LOQs)为2.0μg/kg。在蛋黄酪和松花蛋肠中7种PBs的回收率范围分别为90.0%~99.0%、88.5%~96.0%,相对标准偏差(relative standard deviations,RSDs)分别为不大于7.44%和8.16%。结论此检测方法专属性强、灵敏度好、结果准确,为进出口食品风险筛查提供检测依据。Objective To establish a method for the determination of 7 kinds of parabens(PBs)in egg yolk cheese,preserved eggs sausage by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods Two kinds of samples,egg yolk cheese and preserved eggs sausage,were selected as the research objects.After being hydrolyzed by sodium hydroxide,the samples were extracted with methanol and 20%methanol aqueous solution,centrifuged,and purified and enriched with MAX solid phase extraction column.Kinetex C18 chromatographic column(100 mm×4.6 mm,2.6μm)was used for separation,acetonitrile-5 mmol/L ammonium acetate solution was used as mobile phase,gradient elution,flow rate 0.8 mL/min,and monitoring was carried out in the mode of electric spray ion source anion(ESI)and multi reaction monitoring(MRM),and quantitative analysis was carried out by external standard method.Result The linear range of 7 PBs was 10.0–200.0 ng/mL,with correlation coefficients greater than or equal to 0.9990.The limits of detection(LODs)were 0.6μg/kg,and the limits of quantification(LOQs)were 2.0μg/kg.The recoveries of 7 kinds of PBs in egg yolk cheese and preserved eggs sausage were 90.0%–99.0%and 88.5%–96.0%,respectively,and the relative standard deviations(RSDs)were not more than 7.44%and 8.16%,respectively.Conclusion This detection method has strong specificity,good sensitivity,and accurate results,providing a testing basis for risk screening of imported and exported food.

关 键 词：超高效液相色谱-串联质谱法 对羟基苯甲酸酯 氢氧化钠水解 蛋黄酪 松花蛋肠 

分 类 号：O657.63[理学—分析化学] TS253.7[理学—化学]