超高效液相色谱-串联质谱法测定黄酒和白酒中20种磺酰脲类除草剂

摘要

建立了固相萃取净化，超高效液相色谱-电喷雾-质谱/质谱（UPLC-ESI-MS/MS）同时测定黄酒和白酒中20种磺酰脲类除草剂含量的方法。样品经磷酸调pH值后，PEP固相萃取小柱浓缩净化，UPLC-MS/MS分析测定。以Waters Acquity UPLCTM HSS T3色谱柱为分析柱，乙腈和0.1%（v/v）甲酸水溶液为流动相，采用电喷雾正离子（ESI+）模式电离，多反应监测（MRM）模式检测。结果表明，方法在一定的浓度范围内线性关系良好（相关系数r2＞0.997），其检出限为0.2～3.3μg/L，定量限为0.5～10.0μg/L；平均回收率为70.1%～117.8%，相对标准偏差（RSD）为1.6%～10.5%。该方法样品处理简单，测定快速、准确、灵敏度高，适合黄酒和白酒中磺酰脲类除草剂的快速检测和定量分析。%An ultra performance liquid chromatography-electrospray ionization-tandem mass spectrometric (UPLC-ESI-MS/MS) method had been developed for simultaneous determination of 20 kinds of sulfonylurea herbicides in yellow rice wine/Baijiu(liquor). In the process, pH was adjusted by phosphoric acid, then the samples were extracted with PEP SPE cartridge, and then detected by UPLC-MS/MS. LC separation was performed on a Waters Acquity UPLC system with a HSS T3 column, acetonitrile and 0.1%(v/v) formic acid aqueous solution used as the mobile phase. And the 20 sulfonylurea herbicides were determined in the mode of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM). The calibration curve showed good linearity with the correlation coefficient greater than 0.997. The limit of detection (LOD) was 0.2~3.3μg/L and the limit of quantification (LOQ) was 0.5~10.0μg/L, respectively. The recoveries of the 20 sulfonylurea herbi-cides was in the range of 70.1%~117.8%with relative standard deviations (RSD) in the range of 1.6%~10.5%. Such method was easy, fast, sensitive, and suitable for the qualitative and quantitative confirmation of 20 sulfonylurea herbicides in yellow rice wine/Baijiu(liquor).