同位素内标法-高效液相色谱-串联质谱法测定海产品中的甲醛含量  

Determination of formaldehyde content in seafood by isotope internal standard method-high performance liquid chromatography-tandem mass spectrometry

作　　者：廖艳华[1] 周劭桓[1] 林文斯[1] LIAO Yan-Hua;ZHOU Shao-Huan;LIN Wen-Si(Guangxi Center for Disease Control and Prevention,Nanning 530028,China)

机构地区：[1]广西壮族自治区疾病预防控制中心,南宁530028

出　　处：《食品安全质量检测学报》2020年第19期7063-7068,共6页Journal of Food Safety and Quality

基　　金：广西壮族自治区卫生厅科研课题(Z2014166);广西医疗卫生适宜技术与推广应用项目(S2019066)。

摘　　要：目的建立同位素内标-高效液相色谱-串联质谱法测定海产品中甲醛的分析方法。方法样品经水超声处理,10%三氯乙酸(V/V)溶液沉淀蛋白,正己烷除脂肪净化后,下清液通过2,4-二硝基苯肼衍生,衍生产物经电喷雾离子源电离,多反应监测(multiple reaction monitoring, MRM)模式检测和内标法定量。结果甲醛衍生物的检测线性范围为1.0~50.0ng/mL,相关系数为0.9996,方法检出限为1.0μg/kg。平均加标回收率在71.4%~94.0%之间,相对标准偏差<15.0%。结论该方法前处理简单、快速、有效、准确灵敏,适合于海产品中甲醛的定性、定量检测。Objective To establish a method for determination of formaldehyde content in seafood by isotope internal standard method-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). Methods The sample were pretreated by ultrasonic treatment with water, with precipitation of protein by 10% trichloroacetic acid(V/V), and then purified with hexane. Supernatant was derived with 2,4-dinitrobenzenehydrazin, the derivative product was detected by MS/MS using negative electrospray ionization under the multiple reaction monitoring(MRM) and analyzed by internal standard method. Results The linear ranges for formaldehyde derivatives were 1.0-50.0 ng/mL, with the correlation coefficient 0.9996. The limits of detection were 1.0 μg/kg. The average recoveries were in the range of 71.4%-94.0%, with the relative standard deviations(RSDs) <15.0%. Conclusion This method is simple, rapid, effective, accurate and sensitive. It is suitable for the qualitative and quantitative determination of formaldehyde in marine products.

关 键 词：同位素内标法 衍生 高效液相色谱-串联质谱法 海产品 甲醛 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]