QuEChERS-高效液相色谱法测定苹果中多菌灵和噻菌灵

Determination of carbendazim and probenazole in apple by QuEChERS-high performance liquid chromatography

中文关键词:  固相萃取  QuEChERS  多菌灵  噻菌灵  高效液相色谱  苹果

英文关键词:solid phase extraction  QuEChERS  carbendazim  probenazole  high performance liquid chromatography  apple

中文摘要:

      目的 以固相萃取(solid phase extraction, SPE)、QuEChERS作为前处理方法, 采用高效液相色谱检测苹果中多菌灵和噻菌灵。方法 样品加乙腈、MgSO4、无水NaCl、NaAc提取, 离心, 取上清液加PSA净化, 离心, 取2 mL上清液用氮气吹干, 用1.0 mL流动相溶解后, 经高效液相色谱测定, 外标法定量。结果 多菌灵和噻菌灵在0.5~10 μg/mL范围内线性关系良好, 线性相关系数(r2)均大于0.9999, 在0.50、2.0和10 μg/mL 3个添加水平下, 加标回收率为84.15%~99.28%, 相对标准偏差(relative standard deviations, RSDs)为1.69%~3.40% (n=6), 检出限小于0.1 mg/kg。结论 与SPE法相比, QuEChERS法具有更低的检出限、操作简单快速, 适用于苹果中多菌灵和噻菌灵的检测。

英文摘要:

      Objective With solid phase extraction (SPE) and QuEChERS as pretreatment methods, to detect the carbendazim and probenazole in apples by high performance liquid chromatography. Methods The sample was extracted with acetonitrile, MgSO4, anhydrous NaCl and NaAc and centrifuged. The supernatant was purified with PSA and centrifuged, 2 mL purified solution was concentrated to near dry and dissolved by 1.0 mL mobile phase, then detected by HPLC, and quantified by external standard method. Results Carbendazim and probenazole had good linear relationships in the range of 0.5~10 μg/mL, and the linear correlation coefficients (r2) were all more than 0.9999. The average recoveries were 84.15%~99.28% at the three spiked levels of 0.50, 2.0 and 10 μg/mL, and the relative standard deviations (RSDs, n=6) were in the range of 1.69% to 3.40%. The limits of detection (LODs) were below 0.1 mg/kg. Conclusion Compared with SPE, QuEChERS is found to have lower detection limits, and is simple and rapid, which is suitable for the determination of carbendazim and probenazole in apple.