气相色谱法测定乳酸左氧氟沙星中有机溶剂残留量(1)
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[摘要] 目的：建立乳酸左氧氟沙星中有机溶剂残留量的测定方法。方法：采用毛细管气相色谱法，色谱柱为HP-5毛细管柱(30 m×0.32 mm×0.25 μm)，程序升温技术，用内标对比法分离测定甲磺酸左氧氟沙星的残留溶剂。结果：两种溶剂在各自对应的浓度范围内线性关系良好(r>0.999 6)，平均回收率分别为100.42%、100.24%，RSD分别为0.775%、0.778%，最低检测限为7.1、11.0 ng。结论：该方法灵敏、准确、可靠，适用于本品有机溶剂残留量的检测。
[关键词] 乳酸左氧氟沙星；气相色谱法；有机溶剂；残留量
[中图分类号] R927 [文献标识码] C [文章编号] 1674-4721(2011)11(c)-045-02
Determination of residual organic solvents in levofloxacin lactate by gas chromatography
HUANG Jingyan1, Qiao Jiabin2, MA Huiyan2, SONG Zhichao1, LI Aixing2, WU Chunli2*
1.Henan Institute of Veterinary Drug Centre, Henan Province, Zhengzhou 450008, China; 2.School of Pharmaceutical Sciences of Zhengzhou University, Henan Province, Zhengzhou 450001, China
[Abstract] Objective: To establish a method for determination of residual solvent in levofloxacin lactate. Methods: Residual solvent in levofloxacin mesylate were determined by capillary gas chromatog raphy using a HP-5 capillary column(30 m×0.32 mm×0.25 μm), and a detector of FID, and a direct injection. Results: The 2 solvents showed good linear relationship within a certain concentration range (r>0.999 6). Residual solvents were well separated in the column with the respective mean recovery range of 100.42% and 100.24%. The respective repeatability (RSD) was 0.775% and 0.778%, and the respective detection limits was 7.1 ng and 11.0 ng. Conclusion: The method has been proved to be accurate and sensitive. It is quite suitable for content determination of organic solvents in levofloxacin lactate.
[Key words] Levofloxacin lactate; Gas chromatography; Organic solvent; Residual level
乳酸左氧氟沙星是新一代喹诺酮类合成抗菌药，适用于敏感菌所致的呼吸、消化、泌尿、生殖系统、皮肤软组织及外科、耳鼻喉科、眼科、口腔科的各种急、慢性细菌感染。由于乳酸左氧氟沙星在制剂生产过程中使用了甲醇和正丁醇溶剂，根据《中国药典》2010年版二部附录P残留溶剂测定法的要求，应建立残留溶剂测定方法考察其是否残留，并应符合第三类溶剂残留限度的要求[1]，需对这两种残留溶剂准确定量并作为方法学研究[2-8]，应用外标法测定，方法准确、可靠。
1 仪器与试剂
Agilent 6890N气相色谱仪(HP6890化学工作站)，甲磺酸左氧氟沙星(批号：20091001、20091002、20091003，河南普瑞制药有限公司提供)。乙醇、正丁醇、N，N-二甲基甲酰胺均为分析纯。
2 方法与结果
2.1色谱条件
色谱柱：HP-5毛细管柱(Agilent公司，固定液为(5%)苯基-(95%)甲基聚硅氧烷，规格：30 m×0.32 mm×0.25 μm)；柱温：初始温度50℃，保持5 min，以20℃/min升温至280℃，保持5 min；进样口温度：200℃ ......
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