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《化学分析计量》 2019年第03期
DOI:10.3969/j.issn.1008-6145.2019.03.017
超高效液相色谱-串联质谱法测定香菇中29 种农药残留
李柱梅,王毅红,朱其丛,韩洛利
郑州市农产品质量检测流通中心,郑州 450006 
Determination of 29 pesticide residues in lentinus edodes by ultra performance liquid chromatography-tandem mass spectrometry
LI Zhumei, WANG Yihong, ZHU Qicong, HAN Luoli
Zhengzhou Agricultural Products Quality Inspection and Circulation Center, Zhengzhou 450006, China 
摘要:建立同时测定香菇中29 种农药残留的超高效液相色谱-串联质谱(UPLC-MS/MS) 方法。样品以0.1% 甲酸-乙腈溶液为提取剂,用氨基固相萃取柱净化,经浓缩、复溶后进行测定。采用18 柱分离,以0.1% 甲酸溶液和乙腈作为流动相,多反应监测(MRM) 模式检测,用基质匹配标准溶液外标法定量。29 种农药在各自的质量浓度范围内与其色谱峰面积呈良好的线性关系,相关系数大于0.995,方法检出限为0.000 1~0.002 mg/kg。在0.02,0.05,0.1 mg/kg 3 个浓度水平进行加标回收试验,平均回收率为81.3%~97.9%,测定结果的相对标准偏差为2.0%~8.4%(n=6)。该方法前处理过程简便,检测时间短,测定结果准确稳定,适合大批量香菇样品中多农药残留的检测,对于香菇的市场准入和监测有着积极意义。 
Abstract:In order to detect pesticide residues in lentinous edodes rapidly and effectively, a method was developed for simultaneous determination of 29 pesticide residues by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with 0.1% formic acid-acetonitrile solution, and cleaned up by amino solid phase extraction column. The purified liquid was evaporated and redissolved for detection. The analytes were separated by C18 column, ormic acid solution and acetonitrile solution were used as the mobile phase, and finally detected by multiple reaction monitoring (MRM) mode. Quantification analysis was achieved by external standard method with the matrix matches of standard solution. The mass concerntration of 29 pesticides had good relationship in the linear range with the linear correlation coefficients of more than 0.995. The limits of quantitation for the 29 pesticides ranged from 0.000 1-0.002 mg/kg. The average recoveries at spiked levels of 0.02, 0.05, 0.1 mg/kg ranged from 81.3% to 97.9% with relative standard deviations of 2.0%-8.4%(n=6). The method is suitable for the detection of multi-pesticide residues in large quantities of lentinus edodes samples with the simple pretreatment process, accurate and stable detection results, and the short analysis time. This method has positive significance for market access and monitoring of lentinous edodes. 
关键词:固相萃取;超高效液相色谱-串联质谱;香菇;农药残留 
Keywords:solid phase extraction; ultra performance liquid chromatography tandem mass spectrometry; Lentinous edodes; pesticide residues 
本文引用格式:
李柱梅,王毅红,朱其丛,等. 超高效液相色谱- 串联质谱法测定香菇中29 种农药残留[J]. 化学分析计量,2019,28(3):68-73.
LI Z M,WANG Y H,ZHU Q C,et al. Determination of 29 pesticide residues in lentinus edodes by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chemical analysis and meterage,2019,28(3):68-73. 

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