固相萃取-超高压液相色谱-串联质谱法测定海水中16种磺胺类抗生素残留

杨维英<sup>1</sup>; 叶敏强<sup>1</sup>; 张丽<sup>1</sup>; 孔园园<sup>1</sup>; 张晓霞<sup>2*</sup>

引用本文:	杨维英, 叶敏强，张丽，孔园园，张晓霞.固相萃取-超高压液相色谱-串联质谱法测定海水中16种磺胺类抗生素残留[J].环境监控与预警,2022,14(5):65-70
	YANG Wei-ying, YE Min-qiang, ZHANG Li, KONG Yuan-yuan，ZHANG Xiao-xia.Determination of 16 Sulfonamide Antibiotic Residues in Seawater by Solid Phase Extraction Ultra High Pressure Liquid Chromatography Tandem Mass Spectrometry[J].Environmental Monitoring and Forewarning,2022,14(5):65-70

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固相萃取-超高压液相色谱-串联质谱法测定海水中16种磺胺类抗生素残留
杨维英, 叶敏强，张丽，孔园园，张晓霞^1,2
1. 江苏省连云港环境监测中心，江苏连云港 222001;2. 广东省科学院生态环境与土壤研究所，华南土壤污染控制与修复国家地方联合工程研究中心，广东省农业环境综合治理重点实验室，广东广州 510650

摘要:

利用固相萃取前处理方法，净化和富集海水中的16种磺胺类抗生素，采用超高压液相色谱-串联质谱法进行定性和定量检测，建立了完整的海水中磺胺类抗生素的检测方法，并对质谱条件、液相条件和固相萃取条件进行了优化。实验结果表明，16种磺胺类抗生素在0.1～100μg/L质量浓度范围内线性良好，相关系数均可以达到0.996以上，方法检出限为0.3~1.1 ng/L。对水样进行高、中、低3个质量浓度的加标回收实验，回收率分别为82.3%~125.7%，73.3%~125.1%和75.2%~119.2%，相对标准偏差为2.4%~12.0%。该方法具有操作简便、重现性好、灵敏度高的优点，可用于海水中磺胺类抗生素的监测分析。

关键词: 固相萃取超高压液相色谱-串联质谱磺胺类抗生素海水

DOI：

分类号:X834

基金项目:江苏省环境监测科研基金资助项目（2120）

Determination of 16 Sulfonamide Antibiotic Residues in Seawater by Solid Phase Extraction Ultra High Pressure Liquid Chromatography Tandem Mass Spectrometry

YANG Wei-ying, YE Min-qiang, ZHANG Li, KONG Yuan-yuan，ZHANG Xiao-xia^1,2

1.Lianyungang Environmental Monitoring Center of Jiangsu Province, Lianyungang, Jiangsu 222001, China;2.NationalRegional Joint Engineering Research Center for Soil Pollution Control and Remediation in South China, Guangdong Key Laboratory of Integrated Agroenvironmental Pollution Control and Management, Institute of Ecoenvironmental and Soil Sciences, Guangdong Academy of Sciences, Guangzhou, Guangdong 510650, China

Abstract:

A method for the detection of 16 sulfonamide antibiotic residues in seawater was developed. 16 kinds of sulfonamide antibiotics in seawater were purified and enriched by solid phase extraction(SPE), and ultra high pressure liquid chromatography tandem mass spectrometry(UPLC-MS-MS) were used for qualitative and quantitative analysis. The mass parameters, as well as the liquid chromatographic parameters and SPE conditions were optimized. 16 sulfonamide antibiotics showed a good linear relationship in the concentration range of 0.1～100 μg/L, and the linear correlation coefficients were greater than 0.996. The method detection limits of the target compounds were among 0.3～1.1 ng/L. The recovery rate experiments of high, medium and low concentration levels were carried out, and the recoveries were 82.3%～125.7%, 73.3%～125.1% and 75.2%～119.2%, respectively, with the relative standard deviations in the range of 2.4%～12.0%. The method is simple, reproducible and sensitive. It is suitable for monitoring and analysis of sulfonamides in seawater.

Key words: Solid phase extraction (SPE) Ultra high pressure liquid chromatography tandem mass spectrometry (UPLC-MS-MS) Sulfonamide antibiotics Seawater