摘要
目的建立注射用三磷酸胞苷二钠中辅料甘露醇及精氨酸的测定方法。方法甘露醇测定采用氨基柱,以乙腈-水(6∶1)为流动相,流速1.0 mL·min^-1,采用示差折光检测器(RID)进行检测。精氨酸采用邻苯二甲醛(OPA)为衍生化试剂,C18色谱柱,流动相A为40 mmol·L^-1磷酸二氢钠溶液(用NaOH调节pH至7.8),流动相B为甲醇-乙腈-水(45∶45∶10),梯度洗脱,流速为2.0 mL·min^-1,检测波长为338 nm。结果甘露醇在5~80 mg·mL^-1内与峰面积线性关系良好(r=0.9999),低、中、高浓度回收率均> 99.7%;精氨酸在0.125~2.00 mg·m L^-1内与峰面积线性关系良好(r=0.9997),低、中、高浓度回收率均> 99.0%。结论建立了高效液相色谱-示差折光检测法(HPLC-RID)测定甘露醇及柱前衍生HPLC法测定精氨酸的含量。方法操作简便、灵敏、准确,具有良好的重现性和稳定性,适用于注射用三磷酸胞苷二钠中甘露醇、精氨酸的含量测定。
Objective To determine mannitol and arginine in cytidine disodium triphosphate for injection. Methods Mannitol separation was achieved on an NH2 column with acetonitrile-water(6∶1) as the mobile phase at 1.0 m L·min^-1. RID was used as the detector. Arginine was derived with OPA and separated on a C18 column. Sodium dihydrogen phosphate solution(40 mmol·L^-1)(adjusting pH to 7.8 with NaOH) was used as the mobile phase A, methanol-acetonitrile-water(45∶45∶10) was used as the mobile phase B for the gradient elution at a flow rate 2.0 m L·min^-1, and the detector wavelength at 338 nm. Results There was a good linearity at 5-80 mg·m L^-1 for mannitol(r = 0.9999) and the average recovery was higher than 99.7%. The arginine had a good linearity at 0.125-2.00 mg·mL^-1(r = 0.9997) and the average recovery was higher than 99.0%. Conclusion An HPLC-RID method has been established to determine mannitol and a pre-column derivatization HPLC method to determine arginine. The methods are simple, sensitive, and accurate, and can be used for the content determination of mannitol and arginine in cytidine disodium triphosphate for injection.
作者
郜昭慧
赵璇
周长明
王铁松
游畅
GAO Zhao-hui;ZHAO Xuan;ZHOU Chang-ming;WANG Tie-song;YOU Chang(Beijing Institute for Drug Control Beijing Key Laboratory of Analysis and Evaluation of Chinese Medicine,Beijing 102206)
出处
《中南药学》
CAS
2019年第10期1721-1724,共4页
Central South Pharmacy
关键词
注射用三磷酸胞苷二钠
甘露醇
精氨酸
含量测定
cytidine disodium triphosphate for injection
mannitol
arginine
content determination
