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盐酸大观霉素中杂质检测方案(液相色谱柱)

检测样品 化药制剂

检测项目 限度检查

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Column:TSKgel ODS-100V (I.D.4.6 mm×250 mm, 5μm) Eluent:5 mmol/L ammonium acetate(with TFA to adjust the pH to 3)-ACN(98:2) Flow rate:0.6 mL/min Column Tem.:room temperature Detector:ELSD Detector parameter:gas flow rate:3.5 L/min;Evaporation temperature :50℃ Sample:spectinomycin, concentration:6 mg/ml Injection vol.: 20 μL

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Journal of Separation Science 2011,34,1811-1819 Ec A = actinamine (impurity A); G = tetrahydroxyspectinomycin (impurity G); D = dihydroxyspectinomycin (impurity D); B = actinospectinoic acid (impurity B); S = spectinomycin; F = triol spectinomycin (impurity F); R=(4R)-dihydrospectinomycin; U = unknown impurity; C = (4 S)-dihydrospectinomycin (impurity C). Column:TSKgel ODS-100V (I.D.4.6 mm×250 mm,5um) Eluent: 5 mmol/L ammonium acetate (with TFA to adjust the pHto3) -ACN (98:2) Flow rate: 0.6mL/min Column Tem.: room temperature Detector: ELSD Detector parameter:gas flow rate:3.5 L/min; Evaporation temperature: 50℃ Sample: spectinomycin,concentration: 6 mg/ml Injection vol.: 20 uL

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