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    LC-MS测定双氢青蒿素哌喹片中阿莫西林、头孢克洛和头孢克肟的残留量

    Determination of amoxicillin,cefaclor and cefixime Residues in dihydroartemisinin and piperaquine Phosphate tablets by LC-MS

      摘要
    • 摘要: 目的 建立双氢青蒿素哌喹片中阿莫西林、头孢克洛、头孢克肟残留量的液质联用检测方法。方法 采用Thermo Gold C18色谱柱(2.1 mm×50 mm,1.9 mm);流动相为10 mmol·L-1乙酸铵溶液(A)-乙腈(B)。阿莫西林、头孢克洛稀释剂为10 mmol·L-1乙酸铵溶液(氨水调节pH值至7.2),流速为0.3 mL·min-1,进样量为10 mL;头孢克肟稀释剂为10 mmol·L-1乙酸铵溶液(氨水调节pH值至11.0),流速为0.25 mL·min-1,进样量为2 mL。阿莫西林、头孢克洛和头孢克肟分别采用2种梯度洗脱条件。结果 阿莫西林、头孢克洛和头孢克肟线性良好,线性方程分别为y=3 734.53x-2 188.63(r=0.999 5),y=1 396.67x-266.554(r=0.999 8)和y=3 636.39x+2 277.48(r=0.999 7),重复性RSD分别为3.1%,2.8%,2.2%,回收率分别为107.1%(RSD=4.3%),97.0%(RSD=2.9%),105.8%(RSD=4.4%)。检测限均为2 ng·mL-1。结论 建立的双氢青蒿素哌喹片中阿莫西林、头孢克洛、头孢克肟残留量的液质联用检测方法快速、灵敏、重现性好,可用于该3种成分残留量的检测。

       

      Abstract: OBJECTIVE To establish an LC-MS/MS method for the determination of amoxicillin,cefaclor and cefixime residues in dihydroartemisinin and piperaquine phosphate tablets.METHODS The column was Thermo Gold C18(2.1 mm×50 mm,1.9 mm),mobile phase was 10 mmol·L-1 ammonium acetate solution (A)-acetonitrile (B).The diluent of amoxicillin and cefaclor was 10 mmol·L-1 ammonium acetate solution (adjust the pH value to 7.2 with ammonia),the flow rate was 0.3 mL·min-1,and the injection volume was 10 mL.The diluent of Cefixime was 10 mmol·L-1 ammonium acetate solution (adjust the pH value to 11.0 with ammonia),the flow rate was 0.25 mL·min-1,injection volume was 2 mL.Amoxicillin,cefaclor and cefixime were eluted by 2 gradient conditions respectively.RESULTS The linearity of the method was good,the linear equations were y=3 734.53x-2 188.63(r=0.999 5)(amoxicillin),y=1 396.67x-266.554(r=0.999 8)(cefaclor),y=3 636.39x+2 277.48(r=0.999 7)(cefixime).The repeatability RSDs of amoxicillin,cefaclor and cefacoxime were 3.1%,2.8%,2.2%,respectively.The recovery rates of the three antibiotics were 107.1%,97.0%,105.8%,RSDs were 4.3%,2.9%,4.4%,respectively.The detection limit was 2 ng·mL-1.CONCLUSION The established method for the determination of amoxicillin,cefaclor and cefixime in dihydroartemisinin and piperaquine phosphate tablets by LC-MS is rapid,sensitive and reproducible,which can be used for the determination of the three components.

       

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