超高效液相色谱- 串联质谱法测定干香菇中多菌灵和噻菌灵残留量研究

202 2009, Vol. 30, No. 12

食品科学※分析检测

超高效液相色谱-串联质谱法测定干香菇中

多菌灵和噻菌灵残留量研究

连文浩，苏建峰，江滨炜

(福建华日食品安全检测有限公司，福建 福州 350015)

摘 要：称取1.0g干香菇样品，用0.02mol/L盐酸-甲醇(80:20，V/V)溶液浸泡提取，调节溶液pH值至6～8，用二氯甲烷进行提取净化，旋转蒸发器减压蒸干后，用30%甲醇水溶解，样液用超高效液相色谱分离，电喷雾串联四级杆质谱进行检测，外标法定量。本法研究的多菌灵和噻菌灵的线性范围为1.0～100.0μg/L，线性相关系数R2＞0.99，在1.0～10.0μg/kg的3个添加水平范围内的平均回收率为78%～106%，相对标准偏差为7.9%～9.8%，方法检测限可达1.0μg/kg，在3min内快速完成分析测试，可应用于大通量的实际样品检测。关键词：干香菇；超高效液相色谱-串联质谱法；多菌灵；噻菌灵

Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Carbendazim

and Thiabendazole Residues in Dried Shiitake (Lentinula edodes)

LIAN Wen-hao，SU Jian-feng，JIANG Bin-wei

(Fujian Fairreach Food Safety Testing Co. Ltd., Fuzhou 350015, China)

Abstract ：A method for simultaneous analysis of carbendazim and thiabendazole in dried shiitake was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). Sample was extracted with0.02 mol/L hydrochloric acid solution containing 20% methanol, adjusted pH to 6－8, purified with dichloromethane, dried byrotary evaporator, and dissolved in 30% methanol solution. The sample was detected by the UPLC-MS/MS, and quantified byexternal standard method. Results showed that the linear ranges for determination of carbendazim and thiabendazole by thismethod were both between 1.0 μg/L and 100.0 μg/L (R2 > 0.99); the average recoveries for the two pesticides in dried shiitakespiked at three levels (1.0, 5.0 and 10.0 μg/kg) were 78%－106%, and the RSDs were 7.9%－9.8% (n = 6); the limit of detectionwas 1.0 μg/kg; the method could be quickly finished in 3 min and be applied in large amount detection of samples.

Key words：dried mushroom；ultra-performance liquid chromatography - tandem mass spectrometry (UPLC - MS/MS)；carbendazim；thiabendazole

中图分类号：TS207.53 文献标识码：A 文章编号：1002-6630(2009)12-0202-03

多菌灵(carbendazim)和噻菌灵(thiabendazole)均属苯并咪唑类杀菌剂，是一类高效广谱内吸性杀菌剂，主要用于防治由子囊菌、半知菌和担子菌引起的农作物、果树及经济作物上的多种病害。这类杀菌剂的化学性质稳定，且易渗入农作物体内，耐雨水冲洗，残留时间长，有一定的毒性，因此我国、日本和欧盟都分别对此类杀菌剂规定了最高允许残留限量。目前多菌灵和噻菌灵的常规检测方法有荧光分析法[1-2]、气相色谱法[3-4]、高效液相色谱法[5-7]等，但未见采用超高效液相色谱-串联质谱法(UPLC-MS/MS)对干香菇样品中的多菌灵和噻菌

灵进行检测报道。由于干香菇样品的基质干扰较为复杂，采用一般的分析方法如气相色谱法、液相色谱法在进行干香菇样品中的农药残留检测时始终存在较大的干扰，无法有效将目标分析物与干扰峰进行分离。超高效液相色谱(ultra-performance liquid chromatography，UPLC)是近年兴起的一项全新的液相分离技术，采用1.7μm的填料技术，全面提升了常规液相的分离效率、峰容量和灵敏度，其与质谱的串联更可充分发挥质谱的灵敏度，并大幅缩短检测时间。因此本实验拟采用超高效液相色谱串联三重四级杆质谱技术建立一种高效快

收稿日期：2008-09-02

作者简介：连文浩(1979-)，男，工程师，硕士，主要从事食品安全检测与研究。E-mail：lianwenhao@fairreach.com