目的 建立高效液相色谱串联质谱法测定注射用磺苄西林钠中D(-)型磺苄西林钠含量的方法。方法 采用SHIMADZu VP-ODS色谱柱进行分离,以0.01 mol·L-1乙酸铵溶液-甲醇(90∶10)为流动相,流速为0.6 mL·min-1。在ESI负离子模式下,采用多反应离子监测(MRM)扫描方式进行检测。结果 D(-)型及L(+)型磺苄西林钠能够有效分离。D(-)型磺苄西林钠含量在1.03~51.90 μg·mL-1内与峰面积有良好的线性关系。在3个添加水平下,样品的加标回收率为99.98%,测定结果的相对标准偏差为0.30%(n=9)。结论 MRM方法定量准确、可靠,可用于注射用磺苄西林钠中D(-)型磺苄西林钠的含量检测。
Abstract
To establish a method for determination of D(-) sulbenicillin sodium in sulbenicillin sodium for injection by HPLC/MS. METHODS The analysis was performed on a SHIMADZU VP-ODS column with mobile phase consisting of 0.01 mol·L-1 ammonium acetate solution-methanol (90∶10) at a flow rate of 0.6 mL·min-1. The detection was performed by Multiple Reaction Monitoring (MRM) scanning mode with ESI negative ion mode. RESULTS D(-) and L(+) sulbenicillin could be effectively separated. Good liner relationship was achieved when the concentration of D(-) sulbenicillin was in the range of 1.03-51.90 μg·mL-1(r=0.999 7). The average recovery rate was 99.98% at three levels (RSD=0.30%, n=9). CONCLUSION The MRM method is accurate, reliable, and can be used for the determination of D(-) sulbenicillin sodium in sulbenicillin sodium for injection.
关键词
液质联用 /
注射用磺苄西林钠 /
D(-)型磺苄西林钠 /
含量测定
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Key words
HPLC-MS /
sulbenicillin sodium for injection /
D(-) sulbenicillin /
quantitative analysis
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中图分类号：
R917
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参考文献
[1] YANG Y M, PENG W, ZHANG C Y. Sulbenicillin sodium for injection. China J Mod Med (中国现代医学杂志),2011,21(25):3153-3155.[2] CHANG Y X. Study on synthesis technology of sulbenicillin sodium. TianJin:Tianjin University,2007.[3] LI X K, FAN W, WU Y. Improvement on the synthesis process of D-(-)-α-sulbenicillin disodium. West China J Pharm Sci (华西药学杂志), 2011, 26(4):313-315.[4] SHUAI F W, WANG X F,ZHANG J Y. Purification method of Sulbenicillin sodium:China, 102219793A. 2011-05-04.[5] ZHANG J. Methods of prepare D(-)-sulbenicillin sodium:China, CN101891753A. 2010-08-17.[6] Ch. P(2010) VolⅡ(中国药典2010年版.二部) [S]. 2010: 1139.[7] MA X L,LIU Y M. Determination of related substance and assay method of sulbenicillin sodium by RP-HPLC. Drug Stand China(中国药品标准),2009,10(6):460-463.[8] JI C Y, YANG Q L. Determination of related substances in sulbenicillin by HPLC . Northwest J Pharm (西北药学杂志), 2006, 21(3):103-104.[9] DAI L P, HU L. Determination of related substances in sulbenicillin by HPLC. Chin J Antibiot (中国抗生素杂志), 2008, 33(4):212-214. LIAO M,LI Y,SHU W. Application of multiple reaction monitoring in biomarkers reseach. Journal of Molecular Diagnostics and Therapy(分子诊断与治疗杂志),2010,2(4):275-279.
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脚注
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基金
重大新药创新综合平台临床前药物代谢动力学技术与平台资助项目 (2009ZX09301-012)
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