GC-MS/MS Determination of Residual Amounts of 10 Acidic Herbicides in Tea
摘 要
取茶叶样品5.00 g,用水[预先用50%(体积分数)盐酸溶液调节其酸度至pH 2.0]10.0 mL浸泡30 min。先后用乙腈超声提取2次(每次用乙腈20.0 mL),每次20 min,离心,合并两次提取的上清液,先后于30℃水浴中减压蒸发以及在常温下吹氮至溶液近干,加入乙腈-甲苯-乙酸(75+25+1)混合溶液(简称为ATA混合液)5.0 mL溶解残渣,此溶液流经Cleanert Pestic Carb/NH2固相萃取柱净化。收集流出液(主液),用ATA混合液15.0 mL淋洗萃取柱,收集流出液并与主液合并,在常温条件下吹氮至近干。加入丙酮870 μL溶解残渣。按文献报道的方法进行五氟苄溴(PFBBr)衍生化于60℃水浴中反应1.0 h,用正己烷1.0 mL提取所生成的衍生物。按所选条件用气相色谱-串联质谱法测定提取液中10种酸性除草剂的残留量。结果表明:10种酸性除草剂化合物的质量浓度在一定范围内与其峰面积之间呈线性关系,检出限(3S/N)在0.022 3~1.54 μg·kg-1。以红茶、绿茶和乌龙茶为基质,按标准加入法进行回收试验,回收率在72.2%~109%之间,测定值的相对标准偏差(n=6)在0.10%~5.2%之间。
Abstract
Tea sample (5.00 g) was soaked in 10.0 mL of water[which was adjusted to pH 2.0 with φ 50% HCl solution preliminarily] for 30 min, and extracted ultrasonically twice successively with acetonitrile (20.0 mL for each extraction) for 20 min in each extraction. After centrifugation, the supernatants were collected, combined and evaporated to near-dryness at 30℃ in a water-bath under reduced pressure and further to dryness by N2-blowing at normal temperature. 5.0 mL of a mixture of acetonitrile, toluene and acetic acid (75+25+1, abbreviated as ATA mixture) were added to dissolved the residue, and the solution obtained was purified by passing through the SPE column of Cleanert Pestic Carb/NH2 and the eluate was collected. The SPE column was then eluted with 15.0 mL of the ATA mixture, and the eluate was collected and combined with the first eluate, and the solution was evaporated to near-dryness by N2-blowing under normal temperature. The residue was dissolved in 870 μL of acetone and the 10 acidic herbicides in the solution were derivatized by the PFBBr method in a water-bath at 60℃ for 1.0 h as described in an optimized procedure given in literature. The derivates formed were then extracted from the reaction mixture with 1.0 mL of n-hexane, and in which the derivates were determined by GC-MS/MS method representing residual amounts of the 10 acidic herbicides in the tea sample. As shown by the results, linear relationships between values of peak area and mass concentration of the 10 acidic herbicides were found in the definite ranges, with detection limits (3S/N) in the range of 0.022 3-1.54 μg·kg-1. Test for recovery by standard addition method was made on the base of black tea, green tea and oolong tea, giving results in the range of 72.2%-109%, and RSDs (n=6) ranged from 0.10% to 5.2%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201907004
所属栏目 工作简报
基金项目 国家重点研发计划资助(2018YFC1602800)
收稿日期 2018/6/29
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联系人作者周敏(66871505@qq.com)
备注朱萌萌,工程师,硕士研究生,研究方向为营养与食品安全
引用该论文: ZHU Mengmeng,YE Qun,HU Song,LI Bin,ZHOU Tingting,LIU Xiaoyu,HU Jinfeng,ZHOU Min. GC-MS/MS Determination of Residual Amounts of 10 Acidic Herbicides in Tea[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(7): 762~768
朱萌萌,叶群,胡松,黎斌,周婷婷,刘小羽,胡晋峰,周敏. 气相色谱-串联质谱法测定茶叶中10种酸性除草剂的残留量[J]. 理化检验-化学分册, 2019, 55(7): 762~768
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参考文献
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【14】张莉,桂建业,张永涛,等.改性聚合物萃取-五氟苄基衍生化-气相色谱-质谱法测定水中酚类化合物[J].理化检验-化学分册, 2013,49(10):1155-1158.
【2】GB 2763-2016中国标准书号[S].
【3】张莉,张永涛,桂建业,等.水中氯代酸性除草剂衍生气相色谱法主要要素探讨[J].中国环境监测, 2011,27(4):45-49.
【4】匡华,侯玉霞,储晓刚,等.气相色谱-质谱法同时测定大豆中14种苯氧羧酸类除草剂[J].分析化学, 2006,34(12):1733-1736.
【5】李波,郭德华,韩丽,等.小麦中苯氧羧酸类除草剂残留量的GC-MS/MS研究[J].化学世界, 2005,46(9):524-528.
【6】牛增元,罗忻,汤志旭,等.高效液相色谱-电喷雾串联质谱法快速测定纺织品中苯氧羧酸类除草剂残留量[J].分析化学, 2009,37(4):505-510.
【7】程静,丁磊,蒋俊树,等.液相色谱串联质谱法测定谷物类农产品中苯氧羧酸类除草剂多残留[J].食品科学, 2010,31(20):389-393.
【8】朱昱,谭家镒,孙毓庆.三甲基硅烷衍生化-气相色谱/质谱联用法分析尿中7-氨基硝西泮[J].色谱, 2002,20(5):394-397.
【9】PEREIRO I R, IRIMIA R G, CANO E R, et al.Optimisation of a gas chromatographic-mass spectrometric method for the determination of phenoxy acid herbicides in water samples as silyl derivatives[J]. Analytica Chimica Acta, 2004,524:249-256.
【10】RODRÍGUEZ I, RUBÍ E, GONZÁLEZ R, et al. On-fibre silylation following solid-phase microextraction for the determination of acidic herbicides in water samples by gas chromatography[J]. Analytica Chimica Acta, 2005,537(1/2):259-266.
【11】CSERHÁTI T, FORGÁCS E. Phenoxyacetic acids:Separation and quantitative determination[J]. Journal of Chromatography B:Biomedical Sciences and Applications, 1998,717(1/2):157-178.
【12】LEE P W, AIZAWA H, BAREFOOT A C, et al. Handbook of residue analytical methods for agrochemicals[J]. Prevalence, 2003.
【13】傅得锋,徐豫青.用五氟苄基溴对五氯酚进行衍生化的方法[J].刑事技术, 2002,1(6):15-16.
【14】张莉,桂建业,张永涛,等.改性聚合物萃取-五氟苄基衍生化-气相色谱-质谱法测定水中酚类化合物[J].理化检验-化学分册, 2013,49(10):1155-1158.
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