HPLC法同时测定尼莫地平脂肪乳中溶血磷脂酰胆碱和溶血磷脂酰乙醇胺的含量
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篇名: | HPLC法同时测定尼莫地平脂肪乳中溶血磷脂酰胆碱和溶血磷脂酰乙醇胺的含量 |
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摘要: | 目的:建立同时测定尼莫地平脂肪乳中溶血磷脂酰胆碱(LPC)和溶血磷脂酰乙醇胺(LPE)含量的方法。方法:采用高效液相色谱法。色谱柱为Lichrosher Diol,检测器为蒸发光散射检测器,流动相A为正庚烷-异丙醇溶液(43 ∶ 57,V/V),流动相B为正庚烷-异丙醇-水(29.5 ∶ 59 ∶ 11.5,V/V/V)(梯度洗脱),流速为1.5 ml/min,柱温为40 ℃,进样量为20 μl。结果:LPC和LPE的检测质量浓度线性范围为0.020 0~0.400 0 mg/ml(r=0.999 0)、0.010 0~0.200 0 mg/ml(r=0.999 6),LPC和LPE质量浓度的对数值与其峰面积的对数值线性关系良好;定量限分别为0.013 4、0.013 0 mg/ml,检测限分别为0.007 8、0.007 6 mg/ml;精密度、稳定性、重复性试验的RSD<2%;回收率分别为95.96%~100.63%(RSD=1.83%,n=9)、99.22%~101.76%(RSD=0.80%,n=9)。结论:该方法操作简便,可用于尼莫地平脂肪乳中有关物质的测定。 |
ABSTRACT: | OBJECTIVE: To establish a method for simultaneous determination of lysophosphatidyl choline (LPC) and lysophosphatidyl ethanolamine (LPE) in Nimodipine fat emulsion. METHODS: HPLC was performed on the column of Lichrosher Diol with detector of evaporative light scattering detector with mobile phase A of heptane - isopropyl alcohol solution (43 ∶ 57,V/V), mobile phase B n-heptane - isopropyl alcohol - water (29.5 ∶ 59 ∶ 11.5, V/V/V) (gradient elution) at a flow rate of 1.5 ml/min, column temperature was 40 ℃, and the injection volume was 20 μl. RESULTS: The linear range was 0.020 0-0.400 0 mg/ml for LPC (r=0.999 0) and 0.010 0-0.200 0 mg/ml for LPE (r=0.999 6), and the logarithm value of concentration and peak area showed good linear relationship; the limit of quantitation was 0.013 4 mg/ml for LPC and 0.013 0 mg/ml for LPE; the limit of detection was 0.007 8 mg/ml for LPC and 0.007 6 mg/ml for LPE; RSDs of precision, stability and reproducibility tests were lower than 2%; recoveries were 95.96%-100.63% (RSD=1.83%, n=9) and 99.22%-101.76% (RSD=0.80%,n=9). CONCLUSIONS: The method is simple, and can be used for the determination of related substance in Nimodipine fat emulsion. |
期刊: | 2016年第27卷第24期 |
作者: | 范凯燕,谢依侨,夏自花,杨帆 |
AUTHORS: | FAN Kaiyan,XIE Yiqiao,XIA Zihua,YANG Fan |
关键字: | 高效液相色谱法;尼莫地平脂肪乳;溶血磷脂酰胆碱;溶血磷脂酰乙醇胺;含量测定 |
KEYWORDS: | HPLC; Nimodipine fat emulsion; Lysophosphatidyl choline; Lysophosphatidyl ethanolamine; Content determination |
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