Objective：To establish an HPLC-MS/MS method for simultaneous determination of seven antimicrobial agents (sulfadiazine, pipemidic acid, trimethoprim, sulfamethazine, ofloxacin, norfloxacin and sulfamethoxazole) in adulterated Chinese patent medicines for relieving cough and asthma. Methods：The analysis was performed on a Venusil MP C18 column (4.6 mm×250 mm, 5 μm) with a gradient elution of acetonitrile-methanol (1∶1) -0.3% ammonium formate solution at a flow rate of 1 mL·min-1. The column temperature was 30 ℃. The target compounds were analyzed with LC-MS in two scan modes including full scan MS and full scan MS2. The scan range was m/z 50~650. The drying gas temperature was 325 ℃, the drying gas flow rate was 5 L·min-1, and the drying gas pressure was 103.4 kPa. Results：Sulfadiazine, pipemidic acid, trimethoprim, sulfamethazine, ofloxacin, ofloxacin and sulfamethoxazole were all less than low 0.04 μg and had good linearities in the range of 1.4-17.6 μg•mL-1 (r>0.999 6). The recoveries of high, median, and low concentrations control samples were 94.4%-98.9%. The test result of three batches of negative samples was negative, and the test result of three batches 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.
WANG Yan-hong, WANG Guang-zhu, ZHANG Ren-nan, LIU Fu-sheng, FENG Mei-hui, LI Bing
. Simultaneous determination of adulteration of seven antimicrobial agents in Chinese patent medicines for relieving cough and asthma by HPLC-MS/MS[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(8)
: 1399
-1407
.
DOI: 10.16155/j.0254-1793.2021.08.14
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