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固相萃取—高效液相色谱串联质谱法测定环境水样中14种抗生素 [中文引用][英文引用]

Determination of 14 Antibiotics in Environmental Water Samples Using Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry (SPE-HPLC-MS/MS)

作者:魏志雄  刘丹丹  蓝明雄  王昆鹏  廖瑜  钟玮 
作者(英文):WEI Zhixiong  LIU Dandan  LAN Mingxiong  WANG Kunpeng  LIAO Yu  ZHONG Wei 
单位(英文): 
分类号:R113
出版年·卷·期(页码):2019·9·第5期(502-508)
DOI:
-----摘要:-------------------------------------------------------------------------------------------

目的 建立环境水样中大环内酯类、氟喹诺酮类、林可胺类、β-内酰胺类及四环素类5类共14种抗生素的固相萃取高效液相色谱串联质谱法(SPE-HPLC-MS/MS)的测定方法。方法 处理后的水样使用亲水亲酯(HLB)固相萃取小柱进行目标物富集,以甲醇洗脱,洗脱液氮气吹干复溶,采用HPLC-MS/MS进样分析。以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,CAPCELL PAK C18柱为分析柱,采用电喷雾正离子模式电离,多反应监测模式扫描,外标法定量。结果 14种抗生素分别在(2.0~1 000μg/L浓度范围内,具有良好线性关系,方法检出限分别为(0.1~0.2 ng/L;分别以阴性水样及河水作为基质,14种抗生素的加标平均回收率分别为68.3%~96.1%64.2%~113.3%,相对标准偏差(n=6)分别为1.7%~11.4%1.5%~9.5%;方法应用于东莞市东江水的检测分析,结果检出6种抗生素,质量浓度范围分别为(2.49~46.7 ng/L结论 本法灵敏、准确,可应用于环境水样中多种抗生素的检测。

-----英文摘要:---------------------------------------------------------------------------------------

Objectives An analytical method of solid phase extraction-high performance liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS) was developed for the determination of 14 antibiotics (5 categories) including macrolides, fluoroquinolones, lincosamides, β-lactam and tetracyclines in environmental water samples. Methods Treated water samples were concentrated by solid phase extraction (SPE) through hydrophilic lipophilic balance (HLB) cartridge, eluted by methanol, dried by nitrogen gas and re-dissolved, and analyzed by HPLC-MS/MS. A CAPCELL PAK C18 column was adopted as the analysis column with mobile phases of gradient elution of acetonitrile-0.1% formic acid, the positive ion mode was adopted for electrospray to ionize and the mass spectrometry signal was scanned in multiple reactions monitoring (MRM) mode, the antibiotics were quantified by external standard method. Results The concentrations of 14 antibiotics were in the range of (2.0~1 000) μg/L, showing a good linear relationship with limits of detection of (0.1~0.2) ng/L. The average recoveries of 14 antibiotics from negative water samples and river water samples as substances were in the range of 68.3%~96.1% and 64.2%~113.3%, respectively, and the relative standard deviations (n=6) of 1.7%~11.4% and 1.5%~9.5%, respectively. The developed method was applied in detection and analysis of Dongjiang River in Dongguan. The result showed that six antibiotics were determined with the concentration in the range of 2.49~46.7 ng/L. Conclusions With high sensitivity and good accuracy, the method could be employed in the determination of multiple antibiotics in environmental water samples.

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中文著录格式: 魏志雄,,刘丹丹,,蓝明雄,,王昆鹏,,廖瑜,,钟玮.固相萃取—高效液相色谱串联质谱法测定环境水样中14种抗生素.环境卫生学杂志.2019;9(5):502-508.
英文著录格式: WEI,Zhixiong,,LIU,Dandan,,LAN,Mingxiong,,WANG,Kunpeng,,LIAO,Yu,,ZHONG,Wei.Determination of 14 Antibiotics in Environmental Water Samples Using Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry (SPE-HPLC-MS/MS)..2019;9(5):502-508.

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