QuEChERS净化-液相色谱-串联质谱法测定茶叶中氯噻啉

引用本文: 刘松南, 赵新颖, 董晓倩, 许雯雯, 赵榕. QuEChERS净化-液相色谱-串联质谱法测定茶叶中氯噻啉[J]. 色谱, 2015, 33(11): 1205-1209. doi: 10.3724/SP.J.1123.2015.07006 shu

Citation: LIU Songnan, ZHAO Xinying, DONG Xiaoqian, XU Wenwen, ZHAO Rong. Determination of imidaclothiz in tea by QuEChERS cleanup and liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2015, 33(11): 1205-1209. doi: 10.3724/SP.J.1123.2015.07006 shu

QuEChERS净化-液相色谱-串联质谱法测定茶叶中氯噻啉

刘松南 ^{1,
,} ,
赵新颖 ^2, ,
董晓倩 ^1, ,
许雯雯 ^1, ,
赵榕 ^1,

通讯作者: 刘松南

摘要: 建立了茶叶中农药氯噻啉残留的液相色谱-串联质谱检测方法。茶叶样品用乙腈提取,提取液经QuEChERS法净化,利用PSA(N-丙基乙二胺)、C₁₈、GCB(石墨化炭黑)等吸附剂材料进一步去除杂质,净化液经过离心后取上清液以水等体积稀释。以乙腈-0.1%(v/v)甲酸水溶液为流动相,在0.30 mL/min流速下梯度洗脱,用C₁₈色谱柱进行液相色谱分离,电喷雾正离子模式电离(ESI⁺),选择反应监测(SRM)模式检测,外标法定量。结果表明:氯噻啉在1~500 μ g/L范围内线性关系良好(相关系数r为0.9999),定量限为0.01 mg/kg(S/N≥10),在乌龙茶和绿茶中3个添加水平(0.01、0.3和3 mg/kg)的平均回收率为87.0%~101.0%,相对标准偏差(RSD, n=7)在2.1%~13.1%之间。对多种茶叶的测定结果表明,该方法操作简便、成本低、准确性高、特异性好、分析速度快,可以对茶叶中氯噻啉残留进行定性和定量检测。

关键词:

English

Determination of imidaclothiz in tea by QuEChERS cleanup and liquid chromatography-tandem mass spectrometry

1.
1. Beijing Tea Qualify Supervision and Inspection Station, Beijing 100162, China, ;

Corresponding author: 刘松南

Received Date: 06 July 2015

Abstract: The method for the determination of imidaclothiz residue in tea by liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed. The imidaclothiz in tea was extracted by acetonitrile and purified by QuEChERS with PSA (primary secondary amine), C₁₈, GCB (graphitized carbon black) as the adsorbents. The purified solution was centrifuged and the supernatant was diluted with water of equal volume. The separation was performed on a C₁₈ column with a gradient elution program of acetonitrile (containing 0.1% (v/v) formic acid) and water at a flow rate of 0.30 mL/min. The mass spectrometer was carried out with electrospray ion source in the positive mode (ESI⁺) and selective reaction monitoring (SRM), quantified by external standard solution. The results showed that the mass concentration of imidaclothiz in the range of 1 to 500 μ g/L was linearly correlated with the peak area, and the correlation coefficient (r) was 0.9999. The limit of quantification (LOQ, S/N≥10) was 0.01 mg/kg. The recoveries in oolong tea and green tea at three spiked levels (0.01, 0.3 and 3 mg/kg) varied from 87.0%-101.0% and the relative standard deviations (RSDs, n=7) were between 2.1% and 13.1%. The real sample tests showed that the method is simple, cheap, accurate, specific, rapid, and suitable for the qualitative and quantitative confirmation of imidaclothiz residue in tea.

Key words:

QuEChERS
/ liquid chromatography-tandem mass spectrometry (LC-MS/MS)
/ imidaclothiz
/ tea

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

QuEChERS净化-液相色谱-串联质谱法测定茶叶中氯噻啉

通讯作者: 刘松南

English

Determination of imidaclothiz in tea by QuEChERS cleanup and liquid chromatography-tandem mass spectrometry

Corresponding author: 刘松南

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

QuEChERS净化-液相色谱-串联质谱法测定茶叶中氯噻啉

通讯作者: 刘松南

English

Determination of imidaclothiz in tea by QuEChERS cleanup and liquid chromatography-tandem mass spectrometry

Corresponding author: 刘松南

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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