摘要
目的:建立氨苄西林中苯甲醛残留的测定方法。方法:采用高效液相色谱(HPLC)法,用Ultimate XB-C_(18)(4.6 mm×250 mm,5μm)色谱柱。以0.1%甲酸水溶液为流动相A,以乙腈为流动相B进行梯度洗脱,0~8 min,流动相B 10%-90%;8~10 min,流动相B 90%;10~12 min,流动相B 90%-10%;12~15 min,流动相B 10%,紫外检测器检测波长245 nm,流速1.0 mL/min,柱温40℃。结果:该方法专属性良好,系统干净稳定;苯甲醛在9.89~98.94 ng/mL的范围内,溶液的浓度与峰面积呈良好的线性关系(R^(2)=0.993);检测限为4.95 ng/mL,相当于供试品含量的9.3×10^(-6),定量限为9.89 ng/mL,相当于供试品浓度的18.6×10^(-6);定量限溶液连续进样6针峰面积RSD值为1.0%;方法重复性良好,RSD值为0.3%;精密度的RSD为0.9%(n=12);加标回收率为78.2%~99.0%;溶液在25.5 h内稳定;耐用性良好。结论:本研究建立的方法精密度好,专属性强,可作为氨苄西林中苯甲醛残留量的控制方法。
Objective:To establish a method for determination of benzaldehyde residues in ampicillion.Methods:HPLC method was adocted,the determination was carried out on Ultimate XB-C_(18)column(4.6 mm×250 mm,5μm).The mobile phase A was 0.1%formic acid solution,the mobile B was acetonitrile,linearity gradient elution was as follows:0~8 min,mobile B 10%~90%;8~10 min,mobile B 90%;10~12 min,mobile B 90%-10%;12~15 min,mobile B 10%,at a flow rate of 1.0 mL/min,the ultraviolet detector wavelength was set at 225 nm,and the column temperature was at 40℃.Results:The method has good specificity,the system was clean and stable.In the range of 9.89~98.94 ng/mL,there was a good linear relationship(R^(2)=0.9987)between the concentration of benzaldehyde and the peak area.The detection limit was 4.95 ng/mL,equivalent to 9.3×10^(-6)of the concentration of the test protuct,and the limit of quantitation was 9.89 ng/mL,equivalent to 18.6×10^(-6)of the concentration of the test protuct;the RSD of the limited quantitation solution peak area was 1.0%after 6 consecutive injections.The RSD of repeatability was 0.3%;the RSD of intermediate precision was 0.9%(n=12),with the recoveries ranged from 78.2%to 99.0%;the method has good durability and the solution was stable in 25.5 h.Conclusion:The method is specificity and accurate,and is effective for benzaldehyde residues control in ampicillin.
作者
马璇
司淑贤
李蕊
王艳梅
许鑫
MA Xuan;SI Shuxian;LI Rui;WANG Yanmei;XU Xin(Shandong Lukang Pharmaceutical Co.,Ltd.,Jining 272100,China)
出处
《山东化工》
2025年第12期121-124,127,共5页
Shandong Chemical Industry
关键词
氨苄西林
苯甲醛残留
方法学验证
含量测定
ampicillin
benzaldehyde residues
methodological validation
content determination
