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

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 C_(18)色谱柱(2.1 mm×50 mm,1.9μm);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10μL;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2μL。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。

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 C_(18)(2.1 mm×50 mm,1.9 μm),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 μL.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 μL.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 was2 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.