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

中文关键词:  同位素内标法  衍生  高效液相色谱-串联质谱法  海产品  甲醛

英文关键词:isotope internal standard  derivatization  high performance liquid chromatography-tandem mass spectrometry  seafood  formaldehyde

中文摘要:

      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1.0~50.0 ng/mL, 相关系数为0.9996, 方法检出限为1.0 μg/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。

英文摘要:

      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.