超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法检测婴幼儿配方奶粉中苯并三唑类紫外线吸收剂

Determination of benzotriazole ultraviolet absorbers in infant formula milk powder by ultra performance liquid chromatography-quadrupole- electrostatic field orbitrap high resolution mass spectrometry

中文关键词:  苯并三唑类紫外线吸收剂  婴幼儿配方奶粉  超高效液相色谱-四极杆静电场轨道阱高分辨质谱法

英文关键词:benzotriazole ultraviolet absorbers  infant formulae  ultra performance liquid chromatographyquadrupole-electrostatic field orbitrap high resolution mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法检测婴幼儿配方奶粉中苯并三唑类紫外线吸收剂。方法 样品经乙腈提取, ?20℃冷冻1 h, 离心取上清后上机测定。以ACQUITY UPLC BEH C8色谱柱(100 mm×2.1 mm, 1.7 μm)为分析柱, 甲醇-5 mmol/L乙酸铵为流动相进行梯度洗脱分离, 采用电喷雾电离源正离子模式, 高分辨质谱全扫描模式检测, 基质匹配外标法定量。结果 6种苯并三唑类紫外线吸收剂在0.05~10.00 ng/mL范围内线性关系良好, 相关系数均大于等于0.9977。空白样品的加标回收率为50.39%~109.00%, 相对标准偏差为2.88%~17.99%, 方法检出限为0.01~0.97 ng/g, 定量限为0.04~3.23 ng/g。结论 该方法操作便捷、快速, 能够准确检测婴幼儿配方奶粉中6种苯并三唑类紫外线吸收剂的含量, 对于婴幼儿食品安全监测具有良好的现实意义。

英文摘要:

      Objective To establish a method for the determination of benzotriazole ultraviolet absorbers in infant formulae by ultra performance liquid chromatography-quadrupole-electrostatic field orbitrap high resolution mass spectrometry. Methods The samples were extracted with acetonitrile, frozen at ?20℃ for 1 h, and centrifuged to obtain the supernatant to the machine for determination. The separation was performed on an ACQUITY UPLC BEH C8 column (100 mm×2.1 mm, 1.7 μm) with methanol-5 mmol/L ammonium acetate as mobile phase by gradient elution. The detection was performed with electrospray ionization source in positive ion mode, high resolution mass spectrometry in full scan mode, and quantitative analysis by matrix matched external standard method. Results The line range of 6 kinds of benzotriazole ultraviolet absorbers were good in the range of 0.05?10.00 ng/mL with the correlation coefficients greater than or equal to 0.9977. The recoveries were 50.39%?109.00%, the relative standard deviations were 2.88%?17.99%, the limits of detection and the limits of quantification of the method were 0.01?0.97 ng/g and 0.04?3.23 ng/g, respectively. Conclusion This method is convenient, rapid and capable of accurately detecting the content of 6 kinds of benzotriazole ultraviolet absorbers in infant formulae, which is of good practical significance for the monitoring of infant food safety.