GC-MS测定碳酸司维拉姆中环氧氯丙烷的残留量

Detection of Epichlorohydrin Residue in Sevelamer Carbonate by GC-MS

关键词:  气相色谱-质谱联用法  碳酸司维拉姆  环氧氯丙烷

Key words:  GC-MS  sevelamer carbonate  epichlorohydrin

摘要:

目的 建立气相色谱-质谱联用法测定碳酸司维拉姆中环氧氯丙烷残留量的方法，以满足原料药质量标准中的限度要求。方法 采用DB-17MS毛细管柱（30 m×0.25 mm，0.25 μm）；进样口温度为200℃；离子源温度为230℃；MS四极杆温度为150℃；载气为氦气；柱流量为1.0 mL·min^-1；程序升温；分流比为10：1；定量离子m/z 57。结果 在0.087~0.260 μg·mL^-1内环氧氯丙烷浓度与峰面积呈现良好的线性关系，定量限为0.045 μg·mL^-1，检测限为0.017 μg·mL^-1；平均加样回收率为98.4%。结论 该方法简单快速，专属性强，准确度好，灵敏度高，可以满足碳酸司维拉姆原料药标准中的限度要求。

Abstract:

OBJECTIVE To establish a gas chromatography-mass spectrometry method for the detection of epichlorohydrin in sevelamer carbonate, so as to meet the limit requirements in the quality standard of raw materials. METHODS This method utilized a DB-17MS column(30 m×0.25 mm, 0.25 μm), helium as carrier gas. The inlet temperature was 200℃. Ion source temperatrue was 230℃. MS quadrupole temperature was 150℃. Temperature program was used. The carrier flow was 1.0 mL·min^-1 and split ratio was 10:1. The quantitative ion was m/z 57. RESULTS Epichlorohydrin presented a good linear relationship within the range of 0.087-0.260 μg·mL^-1. The limit of quantitation was 0.045 μg·mL^-1 and the limit of detection was 0.017 μg·mL^-1. The average recovery was 98.4%. CONCLUSION This method is simple and fast, with strong specificity, good accuracy and high sensitivity. It can meet the requirement of limits value of the standard of sevelamer carbonate drug substance.