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采用气相色谱-负化学离子源质谱法(GC-NCI-MS)和气相色谱-串联质谱法(GC-MS/MS)对中国茶叶中的有机氯农药和拟除虫菊酯进行筛查和确证检测

Organochlorine pesticides and pyrethroids in Chinese tea by screening and confirmatory detection using GC-NCI-MS and GC-MS/MS.

作者信息

Zhu Pan, Miao Hong, Du Juan, Zou Jian-hong, Zhang Guo-wen, Zhao Yun-Feng, Wu Yong-Ning

机构信息

Key Laboratory of Food Safety Risk Assessment of Ministry of Health, China National Center for Food Safety Risk Assessment, Beijing, China.

出版信息

J Agric Food Chem. 2014 Jul 23;62(29):7092-100. doi: 10.1021/jf5012424. Epub 2014 Jul 10.

DOI:10.1021/jf5012424
PMID:24964290
Abstract

One hundred and one tea samples including green tea, dark tea, scented tea, black tea, and oolong tea were screened and confirmed for the contamination of 31 organochlorine pesticides (OCPs) and 19 pyrethroids (PYs) by gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS). 50 pesticides, 3 deuterium-labeled PYs, and 24 (13)C-labeled OCPs were separated well with the limits of detection (LODs) ranging from 0.02 to 4.5 μg/kg for GC-NCI-MS, and the positive samples were verified by GC-MS/MS with LODs of 0.1-5.0 μg/kg. High detection rates for some PYs, such as 63.4% for bifenthrin (not detected (ND)-3.848 mg/kg), 55.4% for λ-cyhalothrin (ND-3.244 mg/kg), 46.5% for cypermethrin (ND-0.499 mg/kg), and 24.8% for fenvalerate (ND-0.217 mg/kg), were found in the 101 tea samples. Endosulfan, DDTs, HCHs, and heptachlor, the persistent OCPs, were frequently detected with rates of 63.4% (ND-1.802 mg/kg), 56.4% (ND-0.411 mg/kg), 24.8% (ND-0.377 mg/kg), and 15.8% (ND-0.100 mg/kg), respectively.

摘要

采用气相色谱-负化学电离质谱法(GC-NCI-MS)和气相色谱-串联质谱法(GC-MS/MS),对101份包括绿茶、黑茶、花茶、红茶和乌龙茶在内的茶叶样品进行筛查,以确定其中31种有机氯农药(OCPs)和19种拟除虫菊酯(PYs)的污染情况。50种农药、3种氘代PYs和24种(13)C标记的OCPs在GC-NCI-MS上分离良好,检测限(LODs)为0.02至4.5μg/kg,阳性样品通过GC-MS/MS进行验证,LODs为0.1 - 5.0μg/kg。在101份茶叶样品中,发现某些PYs的检出率较高,如联苯菊酯为63.4%(未检出(ND)- 3.848mg/kg)、高效氯氟氰菊酯为55.4%(ND - 3.244mg/kg)、氯氰菊酯为46.5%(ND - 0.499mg/kg)、氰戊菊酯为24.8%(ND - 0.217mg/kg)。持久性OCPs,如硫丹、滴滴涕、六六六和七氯,检出频率也较高,分别为63.4%(ND - 1.802mg/kg)、56.4%(ND - 0.411mg/kg)、24.8%(ND - 0.377mg/kg)和15.8%(ND - 0.100mg/kg)。

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