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目的:采用固相萃取-毛细管电泳法(SPE-HPCE)同时检测牛奶中磺胺甲噁唑、磺胺甲氧嗪、磺胺氯哒嗪、磺胺对甲氧嘧啶、磺胺间甲氧嘧啶等的含量。方法:以60 mmol·L~(-1)硼砂盐缓冲液(pH 7.32)为电泳介质,运行电压15 kV,压力法进样5 s;柱温15℃;检测波长254 nm。结果:该方法能使5种药物在16 min内得到完全分离,磺胺甲噁唑、磺胺甲氧嗪、磺胺氯哒嗪、磺胺对甲氧嘧啶、磺胺间甲氧嘧啶分别在13.1~104.8 mg·L~(-1)(r=0.999 4),12.8~102.0 mg·L~(-1)(r=0.999 4),14.4~1 15.6 mg·L~(-1)(r=0.999 8),12.7~101.8 mg·L~(-1)(r=0.999 5),和13.7~109.6 mg·L~(-1)(r=0.999 6)的范围内线性关系艮好,平均加样回收率分别为100.8%(RSD=1.5%),101.0%(RSD=1.2%),102.4%(RSD=1.3%),100.9%(RSD=1.9%),104.1%(RSD=0.9%)。结论:本方法简单、可靠,灵敏度高,适用于牛奶中磺胺类药物残留的检测。
OBJECTIVE: To detect the contents of sulfamethoxazole, sulfamethoxine, sulfadiazine, sulfadimethoxine and sulfamonomethoxine in milk by solid-phase extraction-capillary electrophoresis (SPE-HPCE). Methods: 60 mmol·L -1 borax salt buffer (pH 7.32) was used as the electrophoresis medium at a voltage of 15 kV and a pressure of 5 kV for 15 s. The detection wavelength was 254 nm. Results: The method could completely separate the five drugs within 16 min. The contents of sulfamethoxazole, sulfamethoxine, sulfadiazine, sulfadiazine and sulfamonomethoxine were in the range of 13.1-104.8 mg · (-1) (r = 0.999 4), 12.8 ~ 102.0 mg · L -1 (r = 0.999 4) and 14.4 ~ 15.6 mg · L -1 (r = 0.999 8) The linear relationship between 12.7 ~ 101.8 mg · L -1 (r = 0.999 5) and 13.7 ~ 109.6 mg · L -1 (r = 0.999 6) Was 101.0% (RSD = 1.2%), 102.4% (RSD = 1.3%), 100.9% (RSD = 1.9%) and 104.1% (RSD = 0.9%) for 100.8% (RSD = 1.5%). Conclusion: The method is simple, reliable and sensitive. It is suitable for the detection of sulfonamides residues in milk.