摘要
目的：建立HPLC-电喷雾检测器（CAD）检测多烯磷脂酰胆碱注射液中磷脂酰胆碱含量的方法，同时对蒸发光检测器（ELSD）和CAD测定磷脂酰胆碱含量的方法进行比较。方法：采用Lunasilica色谱柱（250mm×4．6mm，5μm），流动相A为甲醇-水-冰醋酸-三乙胺（85：15：0．45：0．05），流动相B为正己烷-异丙醇-流动相A（20：48：32），梯度洗脱，流速1．0mL·min^-1，柱温40℃。ELSD漂移管温度80℃，载气流速2．0L·min^-1；CAD雾化温度30℃，气压0．24MPa。结果：2种检测方法在选定条件下，磷脂酰胆碱与样品中其他组分分离良好，ELSD测定磷脂酰胆碱检测限为0．75μg，在7．5～75．7μg的线性范围内峰面积的对数与质量浓度的对数呈良好的线性关系（r=0．9955），平均回收率（n=9）为100．3％；CAD测定的检测限为0．18μg，在1．5—75．7μg的线性范围内峰面积与质量浓度呈良好的线性关系（r=0．9994），平均回收率（n=9）为100．8％。结论：HPLC—CAD高效、准确，较ELSD线性关系更好，为多烯磷脂酰胆碱注射液提供新的质量控制方法。
Objective： To establish an HPLC - CAD method for the determination of phosphatidylcholine content in polyene phosphatidycholine injection, and to compare HPLC - ELSD and HPLC - CAD methods for the determina- tion of phosphatidylcholine in polyene phosphatidycholine injection. Methods： The Luna silica column （250 mm× 4.6 mm,5 μm） was used. The mobile phase for gradient elution consisted of two eluents ： solvent A was methanol - water - acetic acid - triethylamine （ 85 ： 15 ： 0.45 ： 0. 05 ） and solvent B wash - hexane - 2 - propanol - solvent A （20： 48： 32）. The flow rate was 1.0 mL · min-land the column temperature was 40 ℃. The detector was evapora- tive light -scattering detector（ELSD） with the temperature of drift tube for measurement at 80 ℃, the flow rate of carrier gas 2. 0 L · min-l. The nebulization temperature for the charged aerosol detector（CAD） was maintained at 30 ℃ and the gas pressure was 0. 24 MPa. Results： Under the described condition, phosphatidylcholine was com- pletely separated from other components in polyene phosphatidycholine injection. ELSD determination showed that the LOD of phosphatidylcholine was 0. 75 μg, the linear range was 7.5 -75μg （r = 0. 9955 ）, and the average re- covery（ n =9 ）was 100. 3%. In comparison, CAD determination showed that the LOD of phosphatidylcholine was 0. 18 μg, the linear range was 1.5 - 75.7 μg （ r = 0. 9994）, and the average recovery （ n = 9） was 100. 8 %. Conclu- sion： HPLC- CAD, a new method for phosphatidylcholine analysis,provides high sensitivity and reproducibility. Compared with the HPLC -ELSD method, the CAD method has better linearity, and provides a method for quality control of this kind of injection.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2014年第3期529-533,共5页
Chinese Journal of Pharmaceutical Analysis
