氨苄西林中苯甲醛残留的方法学研究

　　

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-C18 （4.6×250mm，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，0-8min，流动相B 10%-90%；8-10min，流动相B 90%；10-12min，流动相B 90%-10%;12-15min，流动相B 10%，紫外检测器检测波长245nm，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9.89ng/ml-98.94ng/ml的范围内，溶液的浓度与峰面积呈良好的线性关系（R2=0.993）；检测限为4.95ng/ml，相当于供试品浓度的9.3ppm，定量限为9.89ng/ml，相当于供试品浓度的18.6ppm；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25.5h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。
关键词：氨苄西林；苯甲醛残留；方法学验证；含量测定
Methodological research of benzaldehyde residues in ampicillin
Ma Xuan1,Sun Chenchen1,Wang Yanmei1,Xu Xin1
(1.Shandong Lukang Pharmaceutical Co.LTD, Jining 272100, China)
Abstract: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-C18 column(4.6×250mm，5μm). The mobile phase A was 0.1% formic acid solution, the mobile B was acetonitrile, linearity gradient elution was as follows: 0-8min,mobile B 10%-90%;8-10min, mobile B 90%;10-12min, mobile B 90%-10%;12-15min, mobile B 10%, at a flow rate of 1.0mL/min,The ultraviolet detector wavelength was set at 225nm, and the column temperature was at 40℃. Results: The method has good specificity,the system was clean and stable. In the range of 9.89ng/ml-98.94ng/ml,there was a good linear relationship(R2=0.9987)between the concentration of benzaldehyde and the peak area. The detection limit was 4.95ng/ml,equivalent to 9.3ppm of the concentration of the test protuct,and the limit of quantitation was 9.89ng/ml,equivalent to 18.6ppm 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 25.5h. Conclusion: The method is specificity and accurate ,and is effective for benzaldehyde residues control in ampicillin.
Keywords: ampicillin; benzaldehyde residues;methodological validation; content determination

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