高效液相色谱法同时测定止咳平喘类中成药中违规添加的磺胺嘧啶等7种化学抗菌物质  

Simultaneous Determination of Seven Antimicrobial Agents in Adulterated Herbal Medicines for Relieving Cough and Asthma by HPLC-DAD

作　　者：王艳红 李冰[2] 陈真[2] 

机构地区：[1]山东药品食品职业学院,山东威海264210 [2]山东省食品药品检验所,济南250101

出　　处：《中国药学杂志》2014年第8期683-687,共5页Chinese Pharmaceutical Journal

摘　　要：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、诺氟沙星和磺胺甲畦唑。方法采用VenusilMPC18（4．6mm×250mm，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（0～10min，10％A；10～40min，10％A→40％A），流速1mL·min^-1，检测波长280nm，参比波长360nm，波长扫描范围190—400nm，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、诺氟沙星和磺胺甲畦唑在1．4～18．0μg·mL^-1（r=1．0000）、1．4～17．6μg·mL^-1（r=0．9997）、2．4～30．0μg·mL^-1（r=0．9998）、1．5～19．2μg·mL^-1（r=1．0000）、2．6～32．8μg·mL^-1（r=0．9996）、2．0～24．4μg·mL^-1（r=1．0000）、1．4—17．6μg·mL^-1（r=1．0000）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、磺胺甲畦唑。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种化学抗茵物质。OBJECTIVE To establish a method for simultaneous determination of seven antimicrobial agents （ sulfadiazine, pipe- midic acid, trimethoprim, sulfamethazine, ofloxacin, norfloxacin and sulfamethoxazole） in aduherated Chinese patent medicines for re-lieving cough and asthma. METHODS The analysis was performed on a Venusil MP Cls column （4. 6 mm× 250 mm, 5 μm） with a gradient elution （0-10 min, 10% A; 10-40 min, 10% A→40% A） of acetonitrile-methanol（ 1：1 ）（A）-0. 3% ammonium formate solution containing 0. 1% formic acid （B） with a flow rate of 1 mL · min^-1. The detection wavelength was 280 nm, reference wave-length was 360 nm, and the scanning range was from 190 to 400 nm. The column temperature was 30 ℃. RESULTS Sulfadiazine, pipemidic acid, trimethoprim, sulfamethazine, ofloxacin, norfloxacin and sulfamethoxazole had good linearities in the range of 1.4 - 18.0 μg· mL^-1（r=1.0000）, 1.4-17.6 μg· mL^-1（r=0.9997）, 2.4-30.0 μg·mL^-1（r=0.9998）, 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） , respectively. The recoveries of high, median, and low concentrations control samples were 94. 5% - 100. 6% , 90. 3%-98.3% , 93.5%-98.0% , 95.1% - 101.7% , 92. 8% - 103.1% , 93.2% - 100. 9% and 95.5% - 106.3% , respective-ly. The test result of three hatches of negative samples was negative, and the test resuh of three hatches of analog positive samples was positive. Trimethoprim and sulfamethoxazole were found in three batches of counterfeit drugs. CONCLUSION The method can be used for examining seven antimicrobial agents in adulterated Chinese patent medicines.

关 键 词：高效液相-二极管阵列检测器 止咳 平喘 中成药 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 磺胺甲[口恶]唑 

分 类 号：R917[医药卫生—药物分析学]