Citation: DUAN Jie, LI Xing-Hua, LIU Kun, ZHANG Shu-Juan, MA Li, SHI Hong-Mei. Determination of Sulfonamide Residues in Milk by High Performance Liquid Chromatography-Chemiluminescence Method[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(7): 1012-1018. doi: 10.11895/j.issn.0253-3820.170110
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Sulfonamides (SAs), such as sulfaguanidine (SGD), sulfadiazine (SDZ), sulfathiazole (STZ) and sulfamethazine (SMZ), can drastically inhibit the chemiluminescence (CL) intensities generated in both Ag(Ⅲ)-Luminol and Ni(Ⅳ)-Luminol systems. Based on these observations, a novel method of high performance liquid chromatography (HPLC) coupled with CL detection was established. Both the Ag(Ⅲ)-Luminol and Ni(Ⅳ)-Luminol CL systems were employed as detectors, and the performances of the two detecting systems were compared. After separated by HPLC, four SAs reacted with Ag(Ⅲ)-Luminol and Ni(Ⅳ)-Luminol CL system, respectively. Chromatographic conditions were as follows: reversed-phase C18 column (250 mm × 4.6 mm,5 μm), gradient elution, and 0.1% (V/V) formic acid-methanol as mobile phase with flow rate of 1 mL/min. CL conditions were as follows: [Ag(Ⅲ)]=1.4×10-4 mol/L (in 0.12 mol/L NaOH); [Ni(Ⅳ)]=1.5×10-5 mol/L (in 0.12 mol/L NaOH); [Luminol]=1.2×10-7 mol/L; and flow rate=1.0 mL/min. Under the optimal conditions, the detection limits of Ag(Ⅲ)-Luminol CL system were 0.15, 0.96, 1.10, 1.50 μg/mL for SGD, SDZ, STZ, and SMZ, respectively, and the recovery were 81.0%-101.5%. Comparatively, the detection limits of Ni(Ⅳ)-Luminol CL system were 1.5, 17.2, 16.8 μg/mL for SGD, SDZ and STZ, and the recoveries was 83.9%-110.8%. The result showed that the Ag(Ⅲ)-Luminol CL system had a much better performance. The method was applied to the determination of the residues of the above four SAs in milk with satisfactory results.
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