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目的:改进测定门冬氨酸鸟氨酸原料药中有关物质的方法。方法:采用高效液相色谱法。色谱柱为Phenomenex Luna NH2(两根串联),流动相为0.02 mol/L磷酸二氢钾缓冲液(pH 5.6)-乙腈(40 ∶ 60,V/V),流速为1.0 mL/min,检测波长为205 nm,柱温为35 ℃,进样量为20 μL。结果:马来酸、3-氨基-2-哌啶酮、琥珀酸、苹果酸、富马酸、β-门冬氨酰门冬氨酸检测质量浓度线性范围分别为5.398~26.992 μg/mL(r=0.999 1)、5.204~26.021 μg/mL(r=0.999 3)、5.149~25.749 μg/mL(r=0.999 6)、5.174~25.874 μg/mL(r=0.999 3)、5.164~25.823 μg/mL(r=0.999 3)、5.194~25.973 μg/mL(r=0.999 5);定量限分别为0.22、0.53、51.50、103.50、0.26、8.31 ng,检出限分别为0.13、0.26、10.30、20.70、0.13、2.08 ng;精密度、稳定性、重复性试验的RSD均不超过2%;加样回收率分别为99.30%~102.31%(RSD=1.02%,n=9)、99.88%~100.89%(RSD=0.37%,n=9)、99.36%~101.53%(RSD=0.70%,n=9)、99.13%~102.65%(RSD=1.15%,n=9)、100.18%~101.45%(RSD=0.38%,n=9)、99.39%~100.81%(RSD=0.58%,n=9)。6批样品均未检出马来酸、琥珀酸和β-门冬氨酰门冬氨酸;3-氨基-2-哌啶酮含量为0.006%~0.056%,苹果酸含量为0.014%~0.071%,富马酸含量为0.000 5%~0.003 4%,最大未知杂质含量为0.013%~0.110%,未知杂质总含量为0.013%~0.120%。结论:该方法操作简便,精密度、稳定性、重复性均较好,可用于门冬氨酸鸟氨酸原料药中有关物质的测定。
OBJECTIVE: To improve the determination method of related substances in ornithine aspartate raw material. METHODS: HPLC method was adopted. The determination was performed on Phenomenex Luna NH2 column (two series- connected) with mobile phase consisted of 0.02 mol/L potassium dihydrogen phosphate buffer solution (pH 5.6)-acetonitrile (40 ∶ 60, V/V) at the flow rate of 1.0 mL/min. The detection wavelength was set at 205 nm, and column temperature was 35 ℃. The sample size was 20 μL. RESULTS: The linear range of maleic acid, 3-amino-2-piperidinone, succinic acid, malic acid, fumaric acid and β-aspartyl-aspartic acid were 5.398-26.992 μg/mL(r=0.999 1), 5.204-26.021 μg/mL(r=0.999 3), 5.149-25.749 μg/mL (r=0.999 6), 5.174-25.874 μg/mL(r=0.999 3), 5.164-25.823 μg/mL(r=0.999 3), 5.194-25.973 μg/mL(r=0.999 5). The limits of quantitation were 0.22, 0.53, 51.50, 103.50, 0.26 and 8.31 ng; the limits of detection were 0.13, 0.26, 10.30, 20.70, 0.13 and 2.08 ng. RSDs of precision, stability, and reproducibility tests were no more than 2%. The average recoveries were 99.30%-102.31%(RSD=1.02%,n=9), 99.88%-100.89%(RSD=0.37%,n=9), 99.36%-101.53%(RSD=0.70%,n=9), 99.13%-102.65%(RSD=1.15%,n=9), 100.18%-101.45%(RSD=0.38%,n=9), 99.39%-100.81%(RSD=0.58%,n=9). Neither maleic acid, succinic acid and β-aspartyl-aspartic acid were found in 6 batches of samples. The contents of 3-amino-2-piperidinone were 0.006%-0.056%; the contents of malic acid were 0.014%-0.071%; the contents of fumaric acid were 0.000 5%-0.003 4%; the contents of maximal unknown impurity were 0.013%-0.110%; total contents of unknown impurity were 0.013%-0.120%. CONCLUSIONS: The method is simple, precise, stable and reproducible, and can be used for the determination of the related substances in ornithine aspartate raw material.
门冬氨酸鸟氨酸高效液相色谱法马来酸3-氨基-2-哌啶酮琥珀酸苹果酸富马酸β-门冬氨酰门冬氨酸有关物质
Ornithine aspartateHPLCMaleic acid3-amino-2-piperidinoneSuccinic acidMalic acidFumaric acidβ-aspartyl-aspartic acidRelated substance
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