Establishment of the QuEChERS-LC-MS/MS method for high-throughput detection of 12 quinolone residues in chicken

Quinolones (QNs) are a class of antibiotics widely used in livestock and poultry breeding owing to their wide range of antibacterial spectrum and strong antibacterial activity. They are widely used for the prevention and treatment of infectious diseases in animals. However, in practice, issues such as overuse, misuse, and failure to follow withdrawal periods are frequently encountered. This leads to excessive QN residues and their metabolites in animal tissues. Long-term consumption of animal-based foods containing QN residues may lead to the development of pathogen resistance, increase the risk of allergic reactions, and disrupt the gut microbiota, posing a serious threat to human health. Therefore, the issue of QN residues warrants increasing attention. Chicken, a widely consumed meat product in China, makes the monitoring of QN residues particularly important. Establishing an efficient and sensitive detection method for monitoring QN residues in livestock and poultry products is critical.

Efficient and reliable pretreatment techniques are crucial for achieving accurate and stable liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. In this study, a high-throughput detection method based on QuEChERS pretreatment combined with LC-MS/MS is established for the simultaneous determination of 12 QN residues in chicken products. The established QuEChERS-LC-MS/MS method provides a rapid, efficient, sensitive, and reliable analytical approach for routine monitoring, risk assessment, and scientific research on various QN residues in chicken, considerably enhancing detection efficiency. At the same time, a comprehensive validation of the established method is conducted. In accordance with international standards, key parameters such as the linear range, sensitivity, accuracy, precision, and specificity are verified to prove its reliability.

The results show that this method can complete the analysis of 12 QN within 9 minutes. At the 9-minute time point, the standard sample exhibits excellent separation, with symmetrical and sharp chromatographic peaks and no corresponding interference peaks observed near the retention times of the standard sample. The methodological evaluation revealed that the correlation coefficients of the calibration curves were all above 0.9970, the limits of detection value ranged from 0.01 to 0.07 μg/kg, and the limits of quantification value ranged from 0.04 to 0.21 μg/kg. The precision determination results showed that the relative standard deviations (RSDs) of retention times for different concentration standard solutions ranged from 0.03% to 0.27%, whereas the RSDs of peak areas ranged from 1.13% to 4.93%, indicating good instrument precision. The matrix addition experiment showed that the recovery rates of the 12 QN after addition ranged from 91.90% to 108.60%. The higher recovery rate indicates that this method complies with the relevant regulations of the national poultry product quality inspection methods.

This study adopts the advanced QuEChERS sample preparation technique and establishes a rapid determination method for QN residues in chicken, replacing the traditional solid-phase extraction procedure. The method offers fast analysis speed, high sensitivity, good recovery rate, and improved lipid removal efficiency. This simple, rapid, and cost-effective feature can provide guidance for large-scale residue detection experiments, offer strong technical support for poultry meat safety supervision work, and safeguard food safety and human health.