HPLC法测定复方氨基酸注射液(18AA)中胱氨酸与半胱氨酸的含量及其在药品质量评价中的应用

Determination of Cystine and Cysteine in Compound Amino Acid Injection (18AA) by HPLC and Its Application in Drug Quality Evaluation

建立了HPLC法测定复方氨基酸注射液(18AA)中胱氨酸(1)与半胱氨酸(2)的含量。色谱柱采用WatersSunFire C_(18)柱(4.6mm×150mm,3.5μm),流动相A为硫酸铵缓冲液:乙腈(97:3),B为乙腈,梯度洗脱。检测波长为205nm,柱温为40℃,进样量为25μl。结果显示,1和2分别在0.002~0.040mg/ml和0.001~0.027mg/ml内线性关系良好,检测限分别为0.99、0.67μg/ml,平均回收率(n=9)分别为102.3%和100.5%,RSD分别为1.6%和1.5%。处方模拟试验结果显示,样品中1含量低于标示量可能与抗氧剂亚硫酸氢钠的添加有关。建立的方法简便、快速、准确,可为复方氨基酸注射液中1和2的测定提供参考。

An HPLC method was established to determine the content of cystine(1) and cysteine(2) in compound amino acid injection(18AA). The Waters SunFire C_(18) column(4.6 mm×150 mm, 3.5 μm) was used, and the analysis was carried out in the gradient elution mode, with ammonium sulfate buffer∶acetonitrile(97∶3) as mobile phase A, acetonitrile as mobile phase B. The detection wavelength was 205 nm, the column temperature was 40 ℃, and the injection volume was 25 μl. The results showed that it was linear for 1 and 2 in the 0.002-0.040 mg/ml and 0.001-0.027 mg/ml, respectively. The detection limits were 0.99 and 0.67 μg/ml, respectively. The mean recoveries(n=9) of 1and 2 were 102.3% and 100.5%, with the RSDs of 1.6% and 1.5%. The results of the simulation test on the formulation showed that the content of 1 in the sample was lower than the labeled amount, which might be related to the addition of the antioxidant sodium bisulfite. The established method is simple, rapid and accurate, which can provide a reference for the determination of 1 and 2 in compound amino acid injection.