This study aims to establish a modified analytical method with sensitivity and reliability for streptomycin (STP) and dihydrostreptomycin (DHS) of residues level in pig tissues, plasma and urine by LC-MS/MS on the basis of previous studies. The mass parameters of quantitative and qualitative ions for STP and DHS were optimized using multiple reaction monitoring in positive mode. The separation of compounds was conducted using BEH Amide column according to material’s characteristics. The analytes in plasma were extracted with only organic solvents. In muscle and kidney, KH2PO4 buffer solution containing 2% CCl3COOH and EDTA-Na was used as extraction solvent. The WCX cartridege was selected as SPE cartridge in considering high recoveries for STP and DHS. The analytes in urine were extracted by organic solvents with acid and addition of EDTA. The limits of detection (LODs) in STP and DHS ranged 0.45~3.66 μg/kg and 0.22~0.78 μg/kg, respectively. The limits of quantification (LOQs) were 1.35~11.10 μg/kg in STP and 0.66~2.36 μg/kg in DHS. The recoveries (%) were 94.29~104.5% in STP and 92.32~108.45% in DHS except for plasma with lower values (61.45/68.5%, respectively). In the precision evaluation, the coefficient of variation (CV, %) of STP showed <10.50% on intra-day and <18.04% on inter-day. The CV (%) of DHS showed <8.42% on intra-day, whereas <17.98% on inter-day. The modified method is reliable for continuous residual monitoring in pig to ensure food safety for consumer’s health. In addition, this method could be used in study relation to residue depletion and pharmacokinetics of veterinary drug.

A method was developed for the simultaneous detection of an antibiotic fungicide, streptomycin, and its metabolite (dihydrostreptomycin) in agricultural products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted using methanol adjusted to pH 3 using formic acid, and purified with a HLB (Hydrophilic lipophilic balance) cartridge. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.001 to 0.1 mg/kg, and linearity of five agricultural products (hulled rice, potato, soybean, mandarin, green pepper), with coefficients of determination (R2) ≥ 0.9906, for streptomycin and dihydrostreptomycin. The mean recoveries at three fortification levels (LOQ, LOQ × 10, LOQ × 50, n = 5) were from 72.0~116.5% and from 72.1~116.0%, and relative standard deviations were less than 12.3% and 12.5%, respectively. The limits of quantification (LOQ) were 0.01 mg/kg, which are satisfactory for quantification levels corresponding with the Positive List System. All optimized results satisfied the criteria ranges requested in the Codex guidelines and the Food Safety Evaluation Department guidelines. The present study could serve as a reference for the establishment of maximum residue limits and be used as basic data for detection of streptomycin and dihydrostreptomycin in food.