Zhou Xue, Cao Shurui, Li Xianliang, Tang Bobin, Ding Xiaowen, Xi Cunxian, Hu Jiangtao, Chen Zhiqiong
College of Pharmacy, Chongqing Medical University, Chongqing 400016, China.
Chongqing Entry-Exit Inspection and Quarantine Bureau, Chongqing Engineering Technology Research Center of Import and Export Food Safety, Chongqing 400020, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 May 1;989:21-6. doi: 10.1016/j.jchromb.2015.02.030. Epub 2015 Mar 10.
A new method combining dispersive-solid phase purification procedure with ultra high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry was developed for simultaneous determination of 18 preservative residues in vegetables. The new method not only had the advantages of dispersive-solid phase purification procedure such as high recoveries, easy operation, rapid analysis, little solvent usage and wide analysis range of preservatives, but also had the advantages of ultra high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry to be operated in positive mode and negative mode simultaneously. The method was validated for the following representative matrices: radish (tuber), tomato (eggplant fruit), cabbage (leafy), cowpea (bean), cucumber (melon) and so on. Samples were extracted with hexane-ethyl acetate (1:2, v/v), and then detected by ultra high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry after being cleaned up with dispersive-solid phase purification procedure. Significant matrix effects were compensated by using the matrix-matched calibration curves. 18 preservatives showed good linearity over the range of 5.0-100.0 μg/L with correlation coefficients of 0.9904-1.000. The limits of detections were in the range of 0.04-4.16 μg/kg and the limits of quantity were in the range of 0.13-13.85 μg/kg. The recoveries of 18 preservatives ranged from 76.0% to 120.0% with the spiked levels of 2, 4 and 10 μg/kg into homogenized vegetables, and the relative standard deviations (RSDs) ranged from 0.3% to 14.8%. Compared with the reported literatures, the method is more rapid, simple, highly sensitive, reliable and can meet testing requirements of 18 preservative residues in vegetables.
建立了一种将分散固相净化程序与超高效液相色谱-三重四极杆/线性离子阱质谱联用的新方法，用于同时测定蔬菜中的18种防腐剂残留。该新方法不仅具有分散固相净化程序回收率高、操作简便、分析快速、溶剂用量少以及防腐剂分析范围广等优点，还具有超高效液相色谱-三重四极杆/线性离子阱质谱可同时在正模式和负模式下运行的优点。该方法在以下代表性基质上进行了验证：萝卜（块茎）、番茄（茄果）、卷心菜（叶菜）、豇豆（豆类）、黄瓜（瓜类）等。样品用正己烷-乙酸乙酯（1:2，v/v）提取，然后经分散固相净化程序净化后，用超高效液相色谱-三重四极杆/线性离子阱质谱进行检测。采用基质匹配校准曲线补偿显著的基质效应。18种防腐剂在5.0 - 100.0 μg/L范围内线性良好，相关系数为0.9904 - 1.000。检测限在0.04 - 4.16 μg/kg范围内，定量限在0.13 - 13.85 μg/kg范围内。在加标水平为2、4和10 μg/kg的匀浆蔬菜中，18种防腐剂的回收率在76.0%至120.0%之间，相对标准偏差（RSD）在0.3%至14.8%之间。与已报道的文献相比，该方法更快速、简便、高灵敏、可靠，能够满足蔬菜中18种防腐剂残留的检测要求。
