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目的建立高效液相-二极管阵列(HPLC-DAD)法同时检查止咳平喘类中成药中非法添加的磺胺嘧啶、吡哌酸、甲氧苄啶、磺胺二甲嘧啶、氧氟沙星、诺氟沙星和磺胺甲唑。方法采用Venusil MP C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-甲醇(1∶1)为流动相A,0.3%甲酸铵溶液(含0.1%甲酸)为流动相B,梯度洗脱(0~10 min,10%A;10~40 min,10%A→40%A),流速1 mL·min-1,检测波长280 nm,参比波长360 nm,波长扫描范围190~400 nm,柱温30℃。结果磺胺嘧啶、吡哌酸、甲氧苄啶、磺胺二甲嘧啶、氧氟沙星、诺氟沙星和磺胺甲唑在1.4~18.0μg·mL-1(r=1.000 0)、1.4~17.6μg·mL-1(r=0.999 7)、2.4~30.0μg·mL-1(r=0.999 8)、1.5~19.2μg·mL-1(r=1.000 0)、2.6~32.8μg·mL-1(r=0.999 6)、2.0~24.4μg·mL-1(r=1.000 0)、1.4~17.6μg·mL-1(r=1.000 0)内呈良好线性关系,高、中、低浓度的回收率(n=3)为94.5%~100.6%、90.3%~98.3%、93.5%~98.0%、95.1%~101.7%、92.8%~103.1%、93.2%~100.9%、95.5%~106.3%;3批阴性样品结果呈阴性,3批模拟阳性样品结果呈阳性;3批假药中检出甲氧苄啶、磺胺甲唑。结论本方法可用于检查止咳平喘中药制剂中非法添加的7种化学抗菌物质。
Objective To establish an HPLC-DAD method for the simultaneous determination of sulfadiazine, pipemidic acid, trimethoprim, sulfamethazine, ofloxacin, norfloxacin Saturn and Sulfamethoxazole. Methods A Venusil MP C18 (4.6 mm × 250 mm, 5 μm) column was used. The mobile phase A consisted of acetonitrile-methanol (1: 1) and 0.3% ammonium formate (0-10 min, 10% A; 10-40 min, 10% A → 40% A) at a flow rate of 1 mL · min-1 with a detection wavelength of 280 nm and a reference wavelength of 360 nm with a wavelength range of 190-400 nm The column temperature was 30 ℃. Results Sulfadiazine, pipemidic acid, trimethoprim, sulfamethazine, ofloxacin, norfloxacin and sulfamethoxazole were significantly higher in 1.4-18.0 μg · mL -1 (r = 1.000 0), 1.4-17.6 (r = 0.999 7), 2.4-30.0 μg · mL -1 (r = 0.999 8), 1.5-19.2 μg · mL -1 (r = 1.000 0), 2.6-32.8 μg · mL -1 (r = 0.999 6), 2.0-24.4 μg · mL -1 (r = 1.000 0) and 1.4-17.6 μg · mL -1 (r = 1.000 0) The rates (n = 3) were 94.5% to 100.6%, 90.3% to 98.3%, 93.5% to 98.0%, 95.1% to 101.7%, 92.8% to 103.1%, 93.2% to 100.9%, 95.5% to 106.3%, respectively; Batch negative samples were negative, three batches of positive samples were positive; trimethoprim and sulfamethoxazole were detected in three batches of counterfeit drugs. Conclusion This method can be used to check the anti-cough and asthma Chinese medicine preparations illegally added seven kinds of chemical antibacterial substances.