超高效液相色谱-串联质谱法测定梨中多抗·喹啉铜多残留

Determination of polyoxin B and oxine-copper in pear by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  多抗霉素B  喹啉铜  梨  超高效液相色谱-串联质谱法  残留分析

英文关键词:polyoxin B  oxine-copper  pear  ultra performance liquid chromatography-tandem mass spectrometry  residue analysis

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)测定梨中多抗霉素B、喹啉铜多残留的分析方法。方法 喹啉铜在酸性条件下转化为8-羟基喹啉后, 其与多抗霉素B经1%乙酸溶液与甲醇(95:5, V:V)提取、PSA净化后, 超高效液相色谱-串联质谱仪进行检测。结果 多抗霉素B和8-羟基喹啉分别在0.001~0.50 mg/L和0.0001~0.050 mg/L浓度范围内, 基质标准工作液的浓度与响应值均呈良好的线性关系, 相关系数r≥0.999。多抗霉素B和喹啉铜在梨中的添加水平分别为0.010~1.0 mg/kg和0.005~1.0 mg/kg, 多抗霉素B的平均回收率在84%~99%之间, 相对标准偏差最大为5.2%; 喹啉铜平均回收率在78%~88%之间, 相对标准偏差最大为3.4%, 表明该方法的准确度和精密度均符合残留分析的要求。其中多抗霉素B和8-羟基喹啉的方法检出限(limits of detection, LOD)分别为1.0×10?11 g和1.0×10?12 g, 方法定量限(limits of quantification, LOQ)分别为0.010 mg/kg和0.005 mg/kg。 结论 该方法灵敏度较高, 有助于提高多抗霉素B和喹啉铜农药的残留风险监测水平。

英文摘要:

      Objective To establish a method for the determination of polyoxin B and oxine-copper in pear by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods 8-hydroxy quinoline converted from oxine-copper and polyoxin B were extracted with 1% acetic acid solution and methanol (95:5, V:V), purified by PSA, and then detected by ultra liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Results The correlation coefficient (r) was no less than 0.999 within the concentration range of 0.001-0.50 mg/L and 0.0001?0.050 mg/L of polyoxin B and 8-hydroxyquinoline, respectively, which indicated a satisfied linear relation between the areas and the concentrations of two target pesticides. Meanwhile, polyoxin B and oxine-copper were fortified into pear blank samples respectively to carry out the recovery tests. The addition levels of polyoxin B and oxine-copper in pear were 0.010 to 1.0 mg/kg and 0.005 to 1.0 mg/kg. The average recoveries of polyoxin B were ranged from 84% to 99%, and the maximum relative standard deviation was 5.2%. The average recoveries of oxine-copper were ranged from 78% to 88%, and the maximum relative standard deviation was 3.4%. The accuracy and precision were accorded with the request of residue analysis. The limits of detection (LOD) of polyoxin B and 8-hydroxyquinoline were 1.0×10?11 g and 1.0×10?12 g, respectively. Their respective limits of quantification (LOQ) were 0.010 mg/kg and 0.005 mg/kg. Conclusion The method is of higher sensitivity, which is helpful to improve the monitoring level of residual risk of polyoxin B and oxine-copper pesticides.