顶空气相色谱法测定美洛昔康中的3种残留溶剂

目的: 建立顶空气相色谱法测定药物美洛昔康中3种残留溶剂的方法。 方法: 采用DB-624毛细管色谱柱(30 m×0.32 mm,1.8 μm);柱温采取程序升温;进样口温度为230 ℃;FID检测器,检测器温度为250 ℃;顶空进样,平衡温度为130 ℃,平衡时间为30 min;以二甲亚砜为溶剂测定美洛昔康原料药中乙醇、N,N-二甲基甲酰胺、二甲苯的残留量。 结果: 在本文的色谱条件下,各有机溶剂均能得到有效分离,乙醇、N,N-二甲基甲酰胺、二甲苯浓度分别在250~750 μg·mL^-1(r=0.9990)、44~132 μg·mL^-1(r=0.9987)、108.5~325.5 μg·mL^-1(r=0.9993)范围内线性关系良好;平均回收率(n=9)分别为97.2%、101.0%、97.9%,RSD分别为1.7%、2.4%、3.1%。 结论: 本方法简便、快速、准确,可有效检测美洛昔康中的残留溶剂。

Objective: To establish a headspace gas chromatography method for determination of three residual solvents in meloxicam. Methods: The residual solvents in Meloxicam were separated on DB-624 columns (30 m×0.32 mm,1.8 μm) with an FID detector.The injector temperature and the detector temperature were set at 230 ℃ and 250 ℃,respectively.The containers of headspace injector were in equilibrium for 30 min at 130 ℃.The dimethylsulfoxide (DMSO) was used as the solvent. Results: The detected solvents were separated completely.Good linearity of the three solvents were obtained within the range of 250-750 μg·mL^-1(r=0.9990),44-132 μg·mL^-1(r=0.9987),108.5-325.5 μg·mL^-1(r=0.9993),respectively.The average recoveries(n=9) of ethanol,N,N-dimethylformamide,xylene were 97.2%,101.0%,97.9% and the RSDs were 1.7%,2.4%,3.1%,respectively. Conclusion: The established method is simple,rapid,and accurate,which can be used for the determination of residual solvents in meloxicam.

1 WANG Ping(王平),GU Zhen-lun(顾振纶).A new non-steroidal anti-inflammatory drug - Meloxicam(新型非甾体抗炎药—美洛昔康).Chin J New Drug Clin Rem(中国新药与临床杂志),2000,19(6):499
2 CAO Li-hua(曹礼华),ZHANG Dong-juan(张东娟),JIANG Shan-xiang(江善祥).Pharmacological effects,pharmacokinetics and clinical application of selective COX-2 inhibitors - meloxicam(选择性COX-2抑制剂美洛昔康的药理作用、药动学及临床应用). Anim Husb Vet Med(畜牧与兽医),2011,43(7):100
3 JIANG Ling-yan(蒋玲燕),LI Qing(李清),CHEN Xiao-hui(陈晓辉),et al.GC simultaneous determination of four components in houttuynia cordata injection(GC法同时测定鱼腥草注射液中4种成分的含量).Chin J Pharm Anal(药物分析杂志),2011,31(4):664
4 WANG Zun-wen(王尊文),ZHAO Zong-ge(赵宗阁),LUAN Cheng-zhang(栾成章),et al.Determination of residual solvents in revaprazan by headspace GC(顶空气相色谱法测定洛氟普啶中有机溶剂残留量). Chin J Pharm Anal(药物分析杂志),2010,30(7):1245
5 XU Ming-zhe(许明哲),ZOU Wen-bo(邹文博),XUE Jing(薛晶),et al.Headspace GC method determination of residual N,N-dimethylformanide in cefalexin drug substance(顶空气相色谱法测定头孢氨苄原料中的残留N,N-二甲基甲酰胺). Chin J Pharm Anal(药物分析杂志),2010,30(10):1876
6 ChP(中国药典).2010.Vol Ⅱ(二部):Appendix(附录)61,194,610
7 WANG Mei(王梅),XING Zhi-yong(邢志勇),LIU Bing(刘冰),et al.Determination of DMF and dimethyl benzene residual in meloxicam(美洛昔康残留DMF、二甲苯的测定).Qilu Pharm Aff(齐鲁药事),2006,25(8):478