Detection of 8 Kinds of Antibiotics Residue in Milk by On-Line Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Double Focusing
10.19756/j.issn.0253-3820.231398
- VernacularTitle:基于双重聚焦的在线固相萃取-高效液相色谱-串联质谱法检测牛奶中8种抗生素残留
- Author:
Yan HUANG
1
;
Xing ZHANG
;
Ting-Ting JIANG
;
Ya-Wen ZHOU
;
Peng JIANG
;
Tao TANG
;
Hong-Feng YIN
Author Information
1. 浙江福立分析仪器有限公司,台州 317500
- Keywords:
On-line solid phase extraction;
Double focusing;
High performance liquid chromatography-tandem mass spectrometry;
Antibiotics;
Milk
- From:
Chinese Journal of Analytical Chemistry
2024;52(12):1904-1912,中插18
- CountryChina
- Language:Chinese
-
Abstract:
A unique on-line solid phase extraction-high performance liquid chromatography-tandem mass spectrometry(SPE-HPLC-MS/MS)system with double focusing was established by double on-line dilution.The targets were first enriched on the head of SPE column by sample online dilution,and then refocused on the head of analysis column by eluent online dilution.The double focusing of the targets could realize direct large-volume injection for analysis of strong solvent samples without causing peak broadening or distortion.The system was evaluated by sulfamethoxazole that had narrowest and highest peak by the on-line SPE-HPLC-MS/MS system with double focusing compared with the conventional on-line SPE-HPLC-MS/MS system and the on-line SPE-HPLC-MS/MS system with one focusing.The system was uesd for analysis of 8 kinds of antibiotics residues in milk.50 μL milk samples were directly analyzed after protein precipitation.In the on-line SPE stage,the loading solvent,elution solvent,elution flow rate and dilution flow rate were systematically optimized.Under the optimal on-line SPE-HPLC-MS/MS conditions,the method validation was carried out to ensure the accuracy of the proposed method.The results showed that 8 kinds of antibiotics had good linear relationships in their respective linear ranges with correlation coefficients(R2)higher than 0.999.The limits of quantification(LOQ)were 0.013-0.126 μg/kg.The recoveries were 80.6%-103.9%,with relative standard deviations(RSDs)of 0.3%-13.5%.The proposed on-line SPE-HPLC-MS/MS system with double focusing was rapid,sensitive,reliable and easy to use for the direct analysis of complex samples.
