气相色谱-串联质谱法快速测定水果中咪鲜胺及其代谢物2,4,6-三氯苯酚的残留量.pdf

※安全检渊
品学
2015,Vol.36,No.12213
气相色谱-串联质谱法快速测定水果中咪鲜胺
及其代谢物2,4,6-三氯苯酚的残留量
卢俊文,李蓉*,杨芳,黄思允,陈丽斯
(中山出入境检验检疫局,广东中山528403)
摘要:目的:建立基质分散固相萃取-气相色谱-串联质谱法快速测定水果中咪鲜胺及其代谢物2,4,6-三氯苯酚残
留量的方法。方法:采用以乙腈作提取剂、以M-丙基乙二胺和十八烷基硅烷键合硅胶(C1)作为混合固相基质分
散萃取净化剂的前处理方法,并利用气相色谱-串联质谱在多反应离子监测模式条件下进行检测,用基质匹配标准
品的外标法定量。结果:咪鲜胺及其代谢物2,4,6-三氯苯酚在0.004~-0.400mgkg范围内线性关系均良好,相关系数
分别为0.9994和0992;在3个添加水平(0.01、0.02、0.10mgkg)范围内的平均回收率分别为80.1%~101.5%和
79.0%~97.4%,相对标准偏差分别为2.8%~6.8%和2.0%~-6.0%,方法的定量限分别为0.04mg/kg和0.005mg/kg
结论:该方法前处理简单快速、灵敏度高、测定线性范围宽,可用于水果中咪鲜胶及其代谢物2,4,6-三氯苯酚残留
的快速测定。
关键词:气相色谱-串联质谱;基质分散固相萃取;咪鲜胺;2,4,6-三氯苯酚;水果;残留
Rapid Determination of Residues of Prochloraz and Its Metabolite 2, 4,6-trichlorophenol in Fruits Using
Gas Chromatography with Tandem Mass Spectrometry
LU Junwen, LI Rong*, YANG Fang, HUANG Siyun, CHEN Lisi
(Zhongshan Entry-exit Inspection and Quarantine Bureau, Zhongshan 528403, China)
Abstract: Purpose: To develop a rapid method for the determination of residues of prochloraz and its metabolite,
2, 4, 6-trichlorophenol, in fruits using matrix dispersive solid-phase extraction and gas chromatography with tandem mass
spectrometry(gc-ms-ms). Methods Samples were extracted with acetonitrile, cleaned by matrix dispersive solid-phase
extraction using PS A and C, detected by GC-MS-MS under multiple reaction monitoring mode, and quantified by an
external standard method using matr xmatch standard solution. Results: In the linear range of 0.004-0 400m/k,the
correlation coefficients for prochloraz and 2, 4, 6-trichlorophenol were 0.9994 and 0.999 2, respectively. Their average
recoveries at spiked levels of 0.01, 0.02 and 0. 10 mg/kg were 80.1%-101.5% and 79.0%-97 4% with relative standard
deviations of 2.8%-6.8% and 2. 0%-6.0% respectivel an r mis of unan(Q(SN=10)were 0.004and
0.005 mg/kg, respectively. onclusions: The proposed method is simple and sensitive with a wide range of measurement,
and can be suitable for the analysis of prochloraz and 2, 4, 6-trichlorophenol residues in fruits
Key words: gas chromatography with tandem mass spectrometry(gc-ms-ms); matrix dispersive solid-phase extraction,
prochloraz 2,4, 6-trichlorophenol; fruit; residue
中图分类号:TS255.7
文献标志码;A
文章编号:1002-6630(2015)12-0213-05
doi:10.7506/spkx1002-6630-201512040
咪鲜胺化学名称:NM-丙基-N-[2-(2,4,6-三氯苯过抑制麦角甾醇的生物合成,使薗体细胞膜功能受破坏
氧基)乙基]咪唑-1-甲酰胺,又称施保克、菌百克、使而起作用。对多种作物由子囊菌和半知菌引起的病害具
百克、扑霉灵,是英国 Boots公司(现在的德国艾格福有明显的防效,常用于防治柑橘的炭疽病、蒂腐病、青
公司)于1974年合成,1977年推向市场的一种咪唑类广病、绿霉病,香蕉炭疽病、叶斑病及芒果炭疽病,也
谱杀菌剂,具有向顶性传导活性,其作用机理主要是通可用于水果采后处理,防治贮藏期病害。咪鲜胺在环境
收稿日期:201408-20
基金项目:广东检验检疫局科技计划项目(2013GDK27);国家质检总局科技计划项目(2015IK260)
作者简介:卢俊文(1981ー),男,主管药师,学土,研究方向为食品分析及天然植物提取。E- mail: dutylu@163com
通信作者:李蓉(1969-),女,高级工程师,硕士,研究方向为食品安全检测技术。E-mail:lir(@zs.gdciq.gov.cn
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