QuEChERS-气相色谱质谱法快速测定水产品中扑草净残留

马丽莎; 尹怡; 田斐; 谢文平; 单奇; 郑光明; 李丽春; 刘书贵; 戴晓欣; 赵城; 魏琳婷; 林嘉薇

doi:10.12131/20210351

QuEChERS-气相色谱质谱法快速测定水产品中扑草净残留

doi: 10.12131/20210351

1.
中国水产科学研究院珠江水产研究所/农业农村部外来入侵水生生物防控重点实验室/广东省水产动物免疫技术重点实验室，广东广州 510380
2.
中国水产科学研究院南海水产研究所/广东省渔业生态环境重点实验室，广东广州 510300

基金项目: 中国-东盟海上合作基金 (CAMC-2018F)；广东省渔业生态环境重点实验室开放基金 (FEEL-2020-8)

详细信息

作者简介:
马丽莎 (1981—)，女，助理研究员，硕士，从事水产品质量安全与风险评估研究。E-mail: malisha16@163.com

通讯作者:
尹　怡 (1982—)，女，副研究员，硕士，从事水产品质量安全与风险评估研究。E-mail: yin.yi@126.com

中图分类号: TS 254.7
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出版历程
- 收稿日期: 2021-11-26
- 修回日期: 2022-01-20
- 录用日期: 2022-02-07
- 网络出版日期: 2022-03-03
- 刊出日期: 2022-08-05

Rapid determination of prometryn in aquatic products by QuEChERS combined with gas chromatography mass spectrometry

1.
Pearl River Fisheries Research Institute, Chinese Academy of Fishery Sciences/Key Laboratory of Prevention and cortrol for Aquatic Invacve Alien Species, Ministry of Agriculture and Rural Affairs/Key Laboratory of Aquatic Animal Immune Technology of Guangdong Province, Guangzhou 510380, China
2.
South China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences/Guangdong Provincial Key Laboratory of Fishery Ecology and Environment, Guangzhou 510300, China

摘要

摘要: 以QuEChERS作为样品前处理手段，建立测定水产品中扑草净残留的气相色谱-质谱法 (GC-MS)。样品以乙腈-二氯甲烷 (V∶V=8∶2) 混合溶液提取，提取液经吸附剂中性氧化铝、N-丙基乙二胺 (PSA)、纳米二氧化锆结合石墨化炭黑 (GCB) 净化后上机检测，内标法定量。结果显示，扑草净质量浓度介于5~200 μg·L⁻¹线性关系良好，相关系数 (R²) 为0.9999。对草鱼 (Ctenopharyngodon idellus)、鳜 (Siniperca chuatsi)、中国对虾 (Penaeus chinensis)、海参 (Holothuria sp.) 和文蛤 (Meretrix meretrix) 进行4个水平的加标回收实验 (10、20、40和200 µg·kg⁻¹)，方法的加标回收率为85.8%~111.8%，相对标准偏差为1.2%~8.8%，满足GB/T 27404—2008《实验室质量控制规范食品理化检测》中实验室质量控制规范。扑草净的检出限 (LOD, S/N≥3) 和定量限 (LOQ, S/N≥10) 分别为5和10 µg·kg⁻¹。该方法简单、快速、灵敏、净化效果好，能满足水产品中扑草净残留的检测需求。
- 气相色谱质谱法 /
- 扑草净 /
- 水产品 /
- QuEChERS /
- 稳定同位素内标
Abstract: A method was developed for the determination of prometryn in aquatic products by quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction coupled with gas chromatography mass spectrometry. The samples were extracted by acetonitrile-dichloromethane mixture (V:V=8:2) and purified by neutral alumina, zirconium dioxide, PSA and GCB, quantified with internal standard. Good linearity was obtained in the range of 5.00−200 µg·L⁻¹ with the correlation coeficient of 0.9999. The average recoveries were 85.8%−111.8% in Ctenopharyngodon idellus, Siniperca chuatsi, Penaeus chinensis, Holothuria sp. and Meretrix meretrix at four spiked levels of 10, 20, 40 and 200 µg·kg⁻¹ with RSD_S of 1.2%−8.8%, which meets the quality control specifications required in the national standard (GB/T 27404−2008 Criterion on Quality Control of Laboratories-Chemical Testing of Food). The limits of detection (S/N≥3) and quantification (S/N≥10) were 5.0 and 10.0 µg·kg⁻¹, respectively. The method is suitable for the rapid determination of the prometryn residues in aquatic products owing to its advantages of simplicity, sensitivity, accuracy and better purification.
- GC-MS /
- Prometryn /
- Aquatic products /
- QuEChERS /
- Isotope labeled internal standard

HTML全文

图 1 进样口不同温度对扑草净灵敏度的影响

Figure 1. Effect of different temperatures of injection port on sensitivity of prometryn

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图 2 不同提取溶剂提取效果的比较

Figure 2. Comparison of extraction effects of different extraction solvents

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图 3 不同提取溶剂对扑草净回收率的影响

Figure 3. Effects of differents extraction solvent on recoveries of prometryn

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图 4 3种吸附剂净化效果的比较

Figure 4. Comparison of purification effects of three adsorbents

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图 5 虾已净化与未净化基质的提取离子色谱图比较

Figure 5. Comparison of extracted ion diagrams of purified and unpurified shrimp

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图 6 僧帽牡蛎样品提取离子色谱图

Figure 6. Extracted ion chromatograms of S. cucullata

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表 1 水产品中扑草净的加标回收率和相对标准偏差 (N=6)

Table 1. Spiked recoveries and relative standard deviations of aquatic product (N=6)

样品　　　　　 Sample	回收率 Average recovery/%				相对标准偏差 RSD/%
样品　　　　　 Sample	10 μg·kg⁻¹	20 μg·kg⁻¹	40 μg·kg⁻¹	200 μg·kg⁻¹	10 μg·kg⁻¹	20 μg·kg⁻¹	40 μg·kg⁻¹	200 μg·kg⁻¹
海参 Holothuria sp.	107.2	97.2	94.2	103.9	8.3	4.5	4.3	3.1
中国对虾 Penaeus chinensis	88.4	97.2	111.8	101.2	5.5	2.3	5.0	2.1
草鱼 Ctenopharyngodon idellus	86.6	106.4	102.7	100.2	5.6	3.3	8.8	4.1
鳜 Siniperca chuatsi	91.6	95.1	95.3	103.9	7.9	1.2	2.4	1.5
文蛤 Meretrix meretrix	92.2	85.8	101.5	100.0	7.0	3.9	3.7	2.7

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