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

中文关键词:  高效液相色谱-串联质谱  对羟基苯甲酸酯  氢氧化钠水解  蛋黄酪  松花蛋肠  

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  parabens  thermosetting egg products  egg yolk cheese  preserved eggs sausage

中文摘要:

      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, 2.6 μm)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0.6 μg/kg, 定量限(limits of quantitation, LOQs)为2.0 μg/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。

英文摘要:

      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, 2.6 μm) 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 0.6 μg/kg, and the limits of quantification (LOQs) were 2.0 μg/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.