In order to verify the efficacy of biochip technology in the detection of veterinary drug residues in raw milk and to promote its application, 80 common veterinary drugs in raw milk were detected by biochip and confirmed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The results showed that the limit of detection (LOD) of the biochip method met the requirements of the national standard, and the LOD for some veterinary drugs was below the national standard limits. The linear range of the method was wide, with correlation coefficient (r) greater than 0.99. Recoveries for negative samples spiked at 2 × and 4 × LOD concentrations were 70%–130%, with coefficient of variation (CV) of 5%–10%. This method has the advantages of simple pretreatment, short detection period and high sensitivity and is suitable for rapid screening of large quantities of samples. Using the proposed method, 10 of 100 batches of raw milk collected from Shanghai during 2022–2023 were tested positive for veterinary drug residues. Streptomyci was detected in 4 batches at concentration levels of 5.86–10.26 μg/kg, sulfapyridine in 3 batches at 1.09–1.42 μg/kg, sulfamonomethoxine in 2 batches at 1.38–1.46 μg/kg, and avermectin in 1 batch at 1.75 μg/kg. These concentration levels were far lower than the maximum residue limits set by international organizations, an announcement of the Ministry of Agriculture and Rural Affairs, and the national standard. Compared with traditional HPLC-MS/MS, the biochip method has the advantages of high sensitivity, wide linear range and fast detection rate. It can be used as a supplementary means for rapid detection of veterinary drug residues in raw milk, and has high application value.
DE ZAYAS-BLANCO F, GARCÍA-FALCÓN M S, SIMAL-GANDARA J, et al. Determination of sulfamethazine in milk by solid phase extraction and liquid chromatographic separation with ultraviolet detection[J]. Food Control, 2004, 15(5): 375-378. DOI:10.1016/S0956-7135(03)00100-2.
FARRÉ M, PICÓ Y, BARCELÓ D. Application of ultra-high pressure liquid chromatography linear ion-trap orbitrap to qualitative and quantitative assessment of pesticide residues[J]. Journal of Chromatography A, 2014, 1328: 66-79. DOI:10.1016/j.chroma.2013.12.082
ZHAO X T, LIN Q B, SONG H, et al. Development of an immunoaffinity chromatography purification and ultra performance liquid chromatography tandem mass spectrometry method for determination of 12 sulfonamides in beef and milk[J]. Journal of Agricultural and Food Chemistry, 2011, 59(18): 9800-9805. DOI:10.1021/jf202705d.
VIDANARACHCHI J K, LI S J, LUNDH A S, et al. Lipolytic activity on milk fat by Staphylococcus aureus and Streptococcus agalactiae strains commonly isolated in Swedish dairy herds[J]. Journal of Dairy Science, 2015, 98(12): 8560-8564. DOI:10.3168/ids.2015-9559.
CHIANG Y C, TSEN H Y, CHEN H Y, et al. Multiplex PCR anda chromogenic DNA macroarray for the detection of Listeria monocytogens, Staphylococcus aureus, Streptococcus agalactiae, Enterobacter sakazakii, Escherichia coli O157:H7, Vibrio parahaemolyticus, Salmonella spp. and Pseudomonas fuorescens in milk and meat samples[J]. Journal of Microbiological Methods, 2012, 88(1): 110-116. DOI:10.1016/j.mimet2011.10.021.
VERCELLI C, AMADORI M, GAMBINO G, et al. A review on the most frequently used methods to detect antibiotic residues in bovine raw milk[J]. International Dairy Journal, 2023, 144: 105695. DOI:10.1016/j.idairyj.2023.105695.
SUN X Y, ZHAO R N, WANG N, et al. Milk somatic cell count: from conventional microscope method to new biosensor-based method[J]. Trends in Food Science and Technology, 2023, 135: 102-114. DOI:10.1016/j.tifs.2023.03.020.
LI W C, LIAO S Y, TSOU C F. A novel sensing chip with dual-coil inductance for determining raw milk quality[J]. Sensors and Actuators A: Physical, 2016, 241: 96-103. DOI:10.1016/j.sna.2016.01.035.