超高效液相色谱-飞行时间质谱法快速分析测定山药中7种常见杀菌剂

Rapid determination of 7 kinds of common fungicides residue in Chinese yam by ultra performance liquid chromatography-time of flight mass spectrometry

中文关键词:  山药  杀菌剂  超高效液相色谱-飞行时间质谱法

英文关键词:Chinese yam  fungicide  ultra performance liquid chromatography-time of flight mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-飞行时间质谱法检测山药中7种常见杀菌剂的分析方法。方法 样品经乙腈提取, 70 ℃水浴氮吹至近干, 丙酮溶解后, 经超高效液相色谱-飞行时间质谱检测。结果 不同温度(50、70 ℃)水浴实验结果表明70 ℃水浴温度符合实验要求。在正离子模式下, 7种杀菌剂在水-甲醇(均含有0.01%甲酸和5 mmol/L甲酸铵)流动相中都具有较好的响应; 各化合物在0.01~0.40 mg/L范围内线性良好, 相关系数r均大于0.999。3个浓度水平的加标回收实验的回收率为70.75%~108.07%, 相对标准偏差为0.02%~5.01%。结论 该方法操作简单、分析准确, 满足山药中常见杀菌剂的检测要求。

英文摘要:

      Objective To establish a method for determination of 7 kinds of common fungicides residues in Chinese yam by ultra performance liquid chromatography-time of flight mass spectrometry (UPLC-TOF-MS). Methods The sample was extracted by acetonitrile, then it was blown by nitrogen at 70 ℃ water bath to nearly dry. The solution was redissolved with acetone and determined by UPLC-TOF-MS. Results The experimental results of water bath at different temperatures (50, 70 ℃) showed that the temperature of water bath at 70 ℃ met the experimental requirements. In the positive ion mode, the seven fungicides all responded well in the mobile phase of water-methanol (containing 0.01% formic acid and 5 mmol/L ammonium formate). Each compound had good linearity in the range of 0.01?0.40 mg/L, and the correlation coefficients r were greater than 0.999. The recoveries of the 3 concentration levels of the standard addition recovery experiment were 70.75%?108.07%, and the relative standard deviations were 0.02%?5.01%. Conclusion This method is simple and accurate, and can meet the requirement of detecting common fungicides in Chinese yam.