摘要
目的应用LC-MS鉴定乙酰吉他霉素中组分及其水解产物。方法以0.1 mol.L-1乙酸铵溶液-乙腈(35∶65)为流动相,采用D iamonsil C18柱,单四极杆质谱检测器,电喷雾正离子扫描,调节锥孔电压,对各色谱峰进行质谱分析。结果乙酰吉他霉素各组分可基本分离;根据所得到的有关相对分子质量以及碎片峰的信息,对乙酰吉他霉素各组分及其水解产物的结构进行了鉴别。发现国产乙酰吉他霉素的主要组分为乙酰吉他霉素A4,A5;A1,A3和A6,A7,与日本药局方中报道的主要组分相同,但国产乙酰吉他霉素还含有较多的乙酰吉他霉素A13。乙酰吉他霉素效价测定中的水解产物并非吉他霉素。结论LC-MS方法快速、灵敏,专属性强,适合用于多组分抗生素的组分分析。
Aim To identify the components of acetylleucomycin and its hydrolytic products by LC- MS. Methods aeetylleueomyein was separated on a Diamonsil C18 column with 0.1 mol·L^-1 ammonium aeetate-aeetontfile （35：65） as mobile phase. The LC-MS was equipped with an eleetorspray ion source （ESI）, which was set at the positive ion mode, and the mass spectra of each component in chromatogram were obtained with difference cone voltage. Results The components of aeetylleueomyein and its hydrolytic products can be separated by HPLC. The components were identified according to the molecular weight and its major mass fragment ions. The major components identified in domastie aeetylleueomyein were acetylleucomyein A4, A5; aeetylleueomyein A1, A3; aeetylleueomyein A6, A7, and aeetylleueomyein A13. The hydrolytic products of aeetylleueomyein were not kitasamyein, but some non-complete hydrolytic product. Conclusion The method is rapid, sensitive and specific. It＇s suitable to application in the fields of multi-components antibiotics analysis.
出处
《药学学报》
CAS
CSCD
北大核心
2006年第5期476-480,共5页
Acta Pharmaceutica Sinica
