2015•Chinese Journal of ChromatographyRequires access

Determination of five β 2 -agonist residues in pork by ultra-high performance liquid chromatography-tandem mass spectrometry with molecularly imprinted solid phase extraction

Xueliang Zhang, Yunjing Luo, Jie Jiang, Yong Lu, Nan Feng

Open publisher page 1 citations

Abstract

An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method with molecularly imprinted solid phase extraction for the determination of five β2-gonists residues in pork has been developed. After the sample preparation, the ammonium acetate/acetic acid buffer was added, followed by the internal standard and β-glucuronidase/arylsulfatase enzyme. The solution was incubated at 55 °C for 2 h. After adjusting the pH of the solution, it was purified by a molecularly imprinted solid phase extraction column, then analyzed on a BEH C18 column with methanol-0.1% (v/v) formic acid aqueous solution as the mobile phases in gradient elution mode. The MS/MS analysis was in positive ion mode and multiple reaction monitoring mode. The analytes were quantified by the internal standard method. The limits of detection (LODs, S/N = 3) and the limits of quantification (LOQs, S/N = 10) were 0.005-0.009 µg/kg and 0.015-0.025 µg/kg, respectively. In the range of 0-10 µg/kg, the correlation coefficients of linear calibration curves were not less than 0.993 3. At the spiked levels of 0.25, 1.0 and 5.0 µg/kg, the recoveries were 80.4%-92.9% with the relative standard deviations of 1.3%-6.3%. The method is of high sensitivity, good reproducibility, high recovery, and is useful for the simultaneous determination of multiple β2-agonists residues.

About this research paper

What this paper is about

An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method with molecularly imprinted solid phase extraction for the determination of five β2-gonists residues in pork has been developed. After the sample preparation, the ammonium acetate/acetic acid buffer was added, followed by the internal standard and β-glucuronidase/arylsulfatase enzyme. The solution was incubated at 55 °C for 2 h. After adjusting the pH of the solution, it was purified by a molecularly imprinted solid phase extraction column, then analyzed on a BEH C18 column with methanol-0.1% (v/v) formic acid aqueous solution as the mobile phases in gradient elution mode. The MS/MS analysis was in positive ion mode and multiple reaction monitoring mode. The analytes were quantified by the internal standard method. The limits of detection (LODs, S/N = 3) and the limits of quantification (LOQs, S/N = 10) were 0.005-0.009 µg/kg and 0.015-0.025 µg/kg, respectively. In the range of 0-10 µg/kg, the correlation coefficients of linear calibration curves were not less than 0.993 3. At the spiked levels of 0.25, 1.0 and 5.0 µg/kg, the recoveries were 80.4%-92.9% with the relative standard deviations of 1.3%-6.3%. The method is of high sensitivity, good reproducibility, high recovery, and is useful for the simultaneous determination of multiple β2-agonists residues.

Why it matters

OpenAlex reports 1 citations for this work. Citation counts describe recorded attention and do not establish research quality.

Key contribution

A contribution statement is not available in the OpenAlex record.

Method / approach

Method details are not available in the OpenAlex metadata.

Main findings

Findings are not separately available in the OpenAlex metadata.

Limitations

Limitations are not available in the OpenAlex metadata.

Applications

Application details are not available in the OpenAlex metadata.

Available abstract

An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method with molecularly imprinted solid phase extraction for the determination of five β2-gonists residues in pork has been developed. After the sample preparation, the ammonium acetate/acetic acid buffer was added, followed by the internal standard and β-glucuronidase/arylsulfatase enzyme. The solution was incubated at 55 °C for 2 h. After adjusting the pH of the solution, it was purified by a molecularly imprinted solid phase extraction column, then analyzed on a BEH C18 column with methanol-0.1% (v/v) formic acid aqueous solution as the mobile phases in gradient elution mode. The MS/MS analysis was in positive ion mode and multiple reaction monitoring mode. The analytes were quantified by the internal standard method. The limits of detection (LODs, S/N = 3) and the limits of quantification (LOQs, S/N = 10) were 0.005-0.009 µg/kg and 0.015-0.025 µg/kg, respectively. In the range of 0-10 µg/kg, the correlation coefficients of linear calibration curves were not less than 0.993 3. At the spiked levels of 0.25, 1.0 and 5.0 µg/kg, the recoveries were 80.4%-92.9% with the relative standard deviations of 1.3%-6.3%. The method is of high sensitivity, good reproducibility, high recovery, and is useful for the simultaneous determination of multiple β2-agonists residues.

Key concepts: Chromatography, Chemistry, Solid phase extraction, Detection limit, Selected reaction monitoring, Formic acid, Extraction (chemistry), Ammonium acetate

Related papers

Back to paper searchBrowse research topicsOriginal source
Determination of five β 2 -agonist residues in pork by ultra-high performance liquid chromatography-tandem mass spectrometry with molecularly imprinted solid phase extraction — Research Paper | ScholarLens