目的 利用液质联用技术对国产鲑降钙素注射液中的主要降解杂质进行结构鉴定。方法 反相色谱柱为Waters XTerra RP C18(3.0 mm×50 mm, 3.5 μm),流动相为体积比0.05%三氟醋酸(TFA)水溶液(A)/ 乙腈(B)梯度洗脱,流速为0.5 mL·min-1;柱温为40 ℃;检测波长为220 nm。分子排阻色谱(SEC)柱为TSK GEL 2000SWxl (7.8 mm×300 mm,5 μm),流动相为TFA-水-乙腈(0.05∶80∶20),流速为0.7 mL·min-1,柱温为室温,检测波长为220 nm。采用正离子模式采集数据。结果 采用RPLC-MS、SEC-MS方法依次推断出3个主要降解杂质的化学结构。结论 本实验对鲑降钙素注射液的杂质谱分析、质量控制具有重要意义。
Abstract
OBJECTIVE To establish an LC-MS method for identification of the primary degradation impurities in domestic calcitonin salmon injections. METHODS For the RPLC analysis, the separation was performed on Waters XTerra RP C18 column (3.0 mm×50 mm, 3.5 μm) with linear gradient elution using 0.05% aqueous trifluoroacetic acid (A) and acetonitrile (B); the flow rate was 0.5 mL·min-1; the column temperature was 40 ℃; the detection wavelength was set at 220 nm. For the SEC analysis, the separation was performed on TSK GEL 2000SWxl column (7.8 mm×300 mm,5 μm) with mobile phase consisting of TFA-water-acetonitrile(0.05∶80∶20); the flow rate was 0.7 mL·min-1; the column temperature was room temperature; the detection wavelength was set at 220 nm; the main impurities were collected and identified by positive mode. RESULTS The structures of three impurities were elucidated by RPLC-MS and SEC-MS.CONCLUSION The RESULTS of this study can be applied in impurity profile analysis, specification research, and quality control of calcitonin salmon injections.
关键词
鲑降钙素注射液 /
降钙素C /
三硫鲑降钙素 /
脱氢丙氨酸鲑降钙素二聚体 /
降解杂质 /
结构鉴定 /
液质联用
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Key words
calcitonin salmon injection /
calcitonin C /
trisulfur salmon calcitonin /
dehydro-ala-calcitonin dimer /
degradation impurity /
structure indentification /
LC-MS
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中图分类号：
R917
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