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 shu

Determination of Sulfonamide Residues in Milk by High Performance Liquid Chromatography-Chemiluminescence Method

School of Public Health, Hebei Medical University, Shijiazhuang 050017, China

Received Date: 24 February 2017
Revised Date: 20 May 2017

Fund Project: This work was supported by the National Natural Science Foundation of China (No.81273128)

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.
- High performance liquid chromatography,
- Chemiluminescence,
- Silver(Ⅲ) complex,
- Nickel(Ⅳ) complex,
- Sulfonamides
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