液相色谱-串联质谱法快速测定蔬菜中10种保鲜剂残留量  

Determination of 10 antistaling agents in vegetables by liquid chromatography-tandem masss pectrometry

作　　者：王军[1] 代艳娜[1] 黄利英[1] 扎西次旦 陈婷[1] 潘虎[1] 白军平[1] 

机构地区：[1]西藏自治区农牧科学院农业质量标准与检测研究所,拉萨850032

出　　处：《食品安全质量检测学报》2015年第6期2379-2385,共7页Journal of Food Safety and Quality

摘　　要：目的建立蔬菜中三唑酮、嘧菌酯、氰霜唑、氟吗啉、哒螨灵、多菌灵、吡唑嘧菌酯、咪鲜胺、腈菌唑、烯酰吗啉共10种保鲜剂类农药残留检测的液相色谱-电喷雾电离-四极杆质谱检测方法。方法分别通过针泵进样和色谱进样将一定浓度的标样试剂导入质谱仪,调整各级质谱和色谱参数,获取所测化合物的质谱图和离子流图,建立仪器分析方法;蔬菜样品经乙腈提取(同时加入氯化钠),加入等体积甲醇水(V:V=1:1)稀释,正己烷脱色后,经色谱导入质谱进行分析。结果对10种保鲜剂成分进行液相色谱-串联质谱法检测:在1.0~100 ng/mL范围内线性良好(r^2>0.99);以5.0、10.0、50.0 ng/mL浓度水平添加回收率为77.9%~119.3%。结论此方法为一种检测保鲜剂类药物在蔬菜中残留的快速准确的分析方法。Objective To establish a liquid chromatography-ESI-mass spectrometry/mass spectrometry (LC-ESI-MS/MS) method to determine 10 kinds of antistaling agents (triadimefon, azoxystrobin, cyazofamid, flumorph, pyridaben, carbendazim, pyraclostrobin, prochloraz, myclobutanil and dimethomorph) in vegetables. Methods Standard samples were injected into mass spectrometer by needle valve and chromatography, then adjusted the parameters of mass spectrometer and chromatography, and achieved the mass spectrometry and total ion chromatogram of the samples for establishing the method of instrumental analysis.The vegetable samples were extracted by acetonitrile with sodium chloride, diluted with equal volume solution of 1:1 (V:V) methanol and water, hexane was applied to decolorize. The sample with injecting into chromatography was analyzed by mass spectrometry. Results The 10 antistaling agents was detected by LC-ESI-MS/MS at 3 levels (5.0, 10.0, and 50.0 ng/mL), the result showed that the correlation coefficient (r2) was more than 0.99 at 1.0~100 ng/mL and the recoveries were in the range of 77.9%~119.3%, which met the requirements of method for determination of residues. Conclusion This method is suitable for fast and accurate detection of 10 antistaling agents in vegetables.

关 键 词：蔬菜 保鲜剂 电喷雾电离 液相色谱-质谱 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]