牛奶中14种除草剂残留的气相色谱-串联质谱检测方法开发

叶倩; 朱富伟; 王刚; 廖林瀚; 唐雪妹

doi:10.16801/j.issn.1008-7303.2021.0170

牛奶中14种除草剂残留的气相色谱-串联质谱检测方法开发

doi: 10.16801/j.issn.1008-7303.2021.0170

叶倩^{1, 2,},
朱富伟^{1, 2},
王刚^{1, 2},
廖林瀚³,
唐雪妹^{1, 2, ,}

1.
广东省农业科学院农业质量标准与监测技术研究所，广州 510640
2.
农业农村部农产品质量安全风险评估实验室(广州)，广州 510640
3.
广东农科监测科技有限公司，广州 510640

基金项目: 国家重点研发计划(2019YFC1605204)；广东省基础与应用基础研究基金项目(2020A1515010620)；广东省农业科学院科技创新战略专项资金(高水平农科院建设).

详细信息

作者简介:
叶倩，yeqian.liao@foxmail.com

通讯作者:
唐雪妹，xuemeitang@gdaas.cn.

中图分类号: O657.63；TS207
计量
- 文章访问数: 359
- HTML全文浏览量: 105
- PDF下载量: 39
- 被引次数: 0
出版历程
- 收稿日期: 2021-06-24
- 录用日期: 2021-09-12
- 网络出版日期: 2021-11-03
- 刊出日期: 2022-04-01

Development of gas chromatography-tandem mass spectrometry detection method for 14 herbicides residues in milk

YE Qian^{1, 2
,},
ZHU Fuwei^{1, 2},
WANG Gang^{1, 2},
LIAO Linhan³,
TANG Xuemei^{1, 2
, ,}

1.
Institute of Quality Standard and Monitoring Technology for Agro-Products of Guangdong Academy of Agricultural Sciences, Guangzhou 510640, China
2.
Laboratory of Quality and Safety Risk Assessment of Agro-Product (Guangzhou), Ministry of Agriculture and Rural Affairs, Guangzhou 510640, China
3.
Guangdong Agricultural Monitoring Technology Co., Ltd. , Guangzhou 510640, China

Funds: National Key Research and Development Program of China (2019YFC1605204), Natural Science Foundation of Guangdong Province (2020A1515010620), Special Fund for Science and Technology Innovation Strategy (Construction of High-Levelacademy of Agricultural Sciences of Guangdong Province).

摘要

摘要: 建立了同时快速检测牛奶中14种除草剂残留的气相色谱-串联质谱(GC-MS/MS)分析方法。样品采用乙腈提取，无水硫酸镁和无水乙酸钠净化，过0.22 μm有机相滤膜后，目标物采用气相色谱-串联质谱(EI离子源)、多反应监测模式(MRM)检测。结果表明：在0.005~1 mg/L范围内，14种目标除草剂的质量浓度与其相应峰面积间呈良好的线性关系，决定系数(R²)均大于0.9902。在0.01、0.05和0.5 mg/kg 3个添加水平下，14种除草剂的平均回收率为76%~113%，相对标准偏差(RSD)为1.2%~8.6% (n=6)。14种除草剂在牛奶中的定量限(LOQ)均为0.01 mg/kg。该方法准确、灵敏、操作步骤简单，适用于同时快速测定牛奶中14种除草剂的残留量。
- 牛奶 /
- 除草剂 /
- 气相色谱-串联质谱(GC-MS/MS) /
- 农药多残留
Abstract: A gas chromatography-tandem mass spectrometry(GC-MS/MS) method for the simultaneous and rapid determination of 14 herbicides in milk was established. The samples were extracted with acetonitrile, cleaned-up with MgSO₄ and Na₂AC, filtered through 0.22 μm organic filter membrane, and the anlytes were determinated with GC-MS/MS (EI source and MRM mode). The results showed that the calibration curve was linear in the range of 0.005-1 mg/L and determination coefficient (R²) was higher than 0.990 2. The average recoveries of 14 herbicides were 76%-113% and the relative standard deviations (RSD) were 1.2%-8.6% (n=6) when the spiked levels were 0.01, 0.05 and 0.5 mg/kg. The limits of quantitation (LOQ) for 14 herbicides were 0.01 mg/kg. The method is accurate, sensitive, simple, and suitable for the simultaneous and rapid determination of 14 herbicides residues in milk.
- milk /
- herbicides /
- gas chromatography-tandem mass spectrometry (GC-MS/MS) /
- pesticide multi-residues

HTML全文

图 1 牛奶基质中14种除草剂的多反应监测色谱图

Figure 1. Chromatography of 14 herbicides in milk matrix by MRM mode

下载: 全尺寸图片幻灯片

图 2 不同提取溶剂对14种除草剂的提取效果

Figure 2. Extraction effects of 14 herbicides by different extraction solvents

下载: 全尺寸图片幻灯片

图 3 乙腈用量对14种除草剂提取效果的影响

Figure 3. Extraction effects of 14 herbicides by different volumes of acetonitrile

下载: 全尺寸图片幻灯片

图 4 不同净化方式对14种除草剂的净化效果

Figure 4. Purification effect of 14 herbicides by different adsorbents

下载: 全尺寸图片幻灯片

表 1 14种除草剂的CAS号、保留时间、定量和定性离子对及碰撞能量

Table 1. The CAS No., retention time, optimized ion pairs and collision energy for the 14 herbicides

除草剂 Herbicide	CAS 号 CAS No.	保留时间 Retention time/min	定量及定性离子对，m/z Q1/Q3	碰撞电压 CE/V
氯苯胺灵 chlorpropham	101-21-3	8.65	153/125.1^*, 153/90, 127/65.1	10, 25, 25
氟乐灵 trifluralin	1582-09-8	9.06	305.9/264^*, 264/160.1, 264/206.2	5, 15, 5
莠去津 atrazine	1912-24-9	10.64	214.9/58.1^*, 214.9/200.2, 200/122.1	10, 5, 5
二甲吩草胺 dimethenamid	87674-68-8	14.27	230/154.1^*, 154.1/111.1, 232/154.1	10, 10, 10
乙草胺 acetochlor	34256-82-1	14.71	174/146.1^*, 146/131.1, 222.9/132.2	10, 10, 20
甲草胺 alachlor	15972-60-8	15.44	188.1/160.2^*, 160/132.1, 188.1/132.1	10, 10, 15
莠灭净 ametryn	834-12-8	15.66	227/58.1^*, 185/170, 227/170.1	10, 5, 10
扑草净 prometryn	7287-19-6	16.02	226/184.2^*, 199/184.1, 241/184.2	10, 5, 10
异丙甲草胺 metolachlor	51218-45-2	17.73	238/162.2^*, 162.2/133.2, 240/162.2	10, 15, 10
二甲戊灵 pendimethalin	40487-42-1	19.09	251.8/162.2^*, 251.8/161.1, 161.9/161.1	10, 15, 10
丁草胺 butachlor	23184-66-9	20.08	176.1/147.1^*, 188.1/160.2, 160.1/132.1	10, 10, 10
敌草胺 napropamide	15299-99-7	20.18	128/72.1^*, 128/100.1, 271/72.1	5, 10, 15
丙草胺 pretilachlor	51218-49-6	20.45	162.1/147.2^*, 162.1/132.2, 262/202.2	10, 20, 5
除草醚 nitrofen	1836-75-5	20.85	202/139.1^*, 282.9/253, 282.9/202	20, 10, 10
注：^定量离子对。Note: ^indicate quantitative ion.

下载: 导出CSV

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