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建立了高效液相色谱法检查磷酸可待因、磷酸可待因与精氨酸布洛芬复方的有关物质,并采用HPLC-TOF/MS和LC-MS/MS对磷酸可待因及两种复方药物产生的降解产物进行了结构鉴定。色谱柱为C18(250 mm×4.6 mm,5μm),柱温50°C,流速1 mL/min,检测波长245 nm,醋酸铵(0.04 M,用醋酸调pH 6.0)–乙腈(92:8,v/v)为流动相A,乙腈为流动相B,梯度洗脱。磷酸可待因在氧化条件下很不稳定产生了两个N-氧可待因异构体,在碱性破坏中得到了新的杂质,其结构可能为6-羟基-3-甲氧基-17-甲基-7,8-双脱氢吗啡-5-醇。在酸性破坏条件下磷酸可待因和精氨酸布洛芬可发生酯化反应。所建立的HPLC方法灵敏、准确,可有效测定磷酸可待因、磷酸可待因与精氨酸布洛芬复方的有关物质,并对产生的降解产物进行了结构鉴定,为更好的控制磷酸可待因与磷酸可待因复方药物的质量提供了依据。
HPLC-TOF / MS and LC-MS / MS were used to determine the contents of codeine phosphate, codeine phosphate and arginine compound ibuprofen, The degradation products of compound drugs were identified by structure. The chromatographic column was C18 (250 mm × 4.6 mm, 5 μm) with a column temperature of 50 ° C and a flow rate of 1 mL / min. The detection wavelength was 245 nm. Ammonium acetate (0.04 M, pH 6.0 with acetic acid) v / v) as mobile phase A, acetonitrile as mobile phase B, gradient elution. Codeine phosphate, which is very labile under oxidative conditions, produces two N-oxoanalog isomers and new impurities in basic destruction, which may be 6-hydroxy-3-methoxy- 17-methyl-7,8-didehydroporphin-5-ol. Esterification occurs between codeine phosphate and arginine ibuprofen under acidic conditions. The established HPLC method is sensitive and accurate, which can effectively determine the related substances of codeine phosphate, codeine phosphate and arginine ibuprofen compound, and structural identification of the degradation products generated, in order to better control the phosphoric acid Codeine and codeine phosphate compound provide the basis for the quality of medicine.