超高效液相色谱-串联质谱法检测婴幼儿辅助食品中多种兽药残留

Special attention must be paid to children and infants because health issues stemming from a poor immunologic system and low weight make them a vulnerable risk group. Complementary foods for infants and young children, which are a class of special dietary foods, are essential transitional foods for infants from lactation to adaptation to ordinary food. Some complementary foods for infants and young children are of animal origin such as fish, meat, and the liver, which may contain veterinary drug residues. Veterinary drugs are usually small-molecular-weight chemicals that are essential for treating infections, increasing production, and improving animal husbandry. However, abuse of these substances can provoke transfer to the food chain, leading to negative consequences for humans, especially infants and young children. For a more comprehensive safety supervision of infant supplementary foods, a method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed and used for the determination of 50 antibiotics and antivirals (grouped into six categories: fluoroquinolones, sulfonamides, macrolides, nitroimidazoles, chloramphenicols, and antivirals) in complementary foods for infants and young children. The matrix of complementary foods for infants and young children is complex and contains a large number of proteins and lipids, which poses a serious challenge for sample pretreatment. The Captiva EMR-Lipid solid-phase extraction (SPE) column is a new type of product that allows for selective and efficient lipid/matrix removal without negatively affecting the recovery of the analyte. In this study, samples were extracted with acidified acetonitrile and then purified using a Captiva EMR-Lipid SPE column. The target analytes were separated on a BEH C18 column by gradient elution using acetonitrile and water containing 0.1% (v/v) formic acid as the mobile phases. MS detection was performed with an electrospray source in the positive and negative modes in the multireaction monitoring (MRM) mode. The ion spray voltages were set at 5500 V and -4500 V in the positive and negative modes, respectively. The source temperature for both the ionization modes was set to 500 ℃. Instrumental parameters such as collision energy and declustering potential were optimized. The samples were quantified using the external standard method with matrix calibration curves to reduce the influence of the matrix effect on the quantitative results. The results showed that the 50 veterinary drug residues had good linear relationships in the range of 0.5 to 50 μg/L, with correlation coefficients higher than 0.995. The limits of detection (LODs) and quantification (LOQs) were in the range of 0.03-0.70 μg/kg and 0.09-2.33 μg/kg, respectively. The average recoveries for all the compounds under different matrices ranged from 64.37% to 119.3% at spiked levels of 5 μg/kg and 50 μg/kg, with relative standard deviations of less than 15%. Compared to QuEChERS, this method has a better purification effect. The recoveries of the 50 veterinary drugs extracted by this method were also much higher than those in the case of QuEChERS. This method was applied to the detection of 14 domestic and six imported infant supplementary foods. Sulfaquinoxaline, sulfamethazine, and tilmicosin were detected in one imported meat-based baby food. With its simple operation, high sensitivity and accuracy, and low sample quantity consumption, this method is suitable for the determination of multiveterinary drug residues in complementary foods for infants and young children. This study provides an effective analysis method for risk monitoring and troubleshooting of complementary foods for infants and young children, which is of great significance in ensuring the healthy growth of the next generation.