Rapid ultra-high performance liquid chromatography-mass spectrum testing method for rifampicin residues in aquatic products

Abstract

The invention discloses a rapid ultra-high performance liquid chromatography-mass spectrum testing method for rifampicin residues in aquatic products. The method comprises the following steps: extracting a sample, purifying the sample, preparing a standard rifampicin concentration gradient working solution with a rifampicin stable isotope interior label; testing the standard rifampicin concentration gradient working solution with the stable isotope interior label of rifampicin and a sample liquid to be tested under identical chromatography and mass spectrum conditions in sequence; acquiring quantitative ion pair and qualitative ion pair information of rifampicin in a multi-reaction monitoring modes (MRM) of tandem quadrupole mass spectrometry; by taking a peak area ratio of rifampicin quantitative ion pairs to rifampicin stable isotope interior label standard substance ion pairs extracted through multi-reaction monitoring as a longitudinal coordinate, and a mass concentration of rifampicin as a transverse coordinate, performing linear regression analysis, introducing the peak area ratio of sample rifampicin to an interior label standard substance into a linear equation, thereby obtaining the content of a target substance in a sample.

Description

Technical field [0001] The invention belongs to the technical field of aquatic product detection, and specifically relates to an ultra-high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) rapid determination method suitable for rifampicin drug residues in aquatic products. Background technique [0002] Rifampicin (CAS: 13292-46-1) is a semi-synthetic antibiotic obtained by chemical modification of rifamycin B. It belongs to the ANSA antibiotics and has a broad-spectrum antibacterial effect. It can be used for It treats a variety of bacterial infectious diseases, and has no cross-resistance with other drugs. It has a particularly outstanding effect on tuberculosis and is a first-line human drug for the treatment of tuberculosis. Rifampicin is a banned drug for veterinary use. The Ministry of Agriculture Announcement No. 560 issued by my country in 2005 has included it in the veterinary drug abolition catalog. However, rifampicin is cheap, has good antibacter...

AI Technical Summary

Problems solved by technology

The method of Jing Jing et al. uses the drug zaleplon as the internal standard for the determination of rifampicin. The chromatographic retention time of the internal standard is quite different from that of rifampicin. The calibration value of the matrix effect is easy to deviate, so it is not necessarily applicable to other substances except plasma. biological matrix

In addition, according to the EU EC / 657 / 2002 regulation that mass spectrometry requires four identification points (IP) for accurate and qualitative detection, the above method only has a pair of ion pairs with m / z 823.4>791.4, and only gets 2 points. Positive risk is higher

At present, there is no report on the detection method of rifampicin residues in aquatic products by liquid chromatography-tandem mass spectrometry. There are many kinds of biological matrices in aquatic products and complex, and the existing rifampicin detection methods cannot meet their detection needs.

The responsibility for food safety issues is heavy, and the lack of accurate and effective rifampicin detection technology has brought great difficulties to the relevant supervision work. Therefore, it is of great practical significance to establish a stable, reliable and accurate method for the determination of rifampicin in aquatic products

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