作者：谢红英1, 雍智全2, 王梦丽1, 冯亚男1, 孙嘉茵1, 李宇茜1, 徐小平1
作者单位：1. 四川大学华西药学院, 四川 成都 610041;
2. 东莞达信生物科技有限公司, 广东 东莞 523808
关键词：正丁胺;离子色谱法;含量测定;系统组织工程技术
摘要：
该文采用系统组织工程技术（ZTSO）快速优化并建立正丁胺含量测定的离子色谱法。选用AcelaimTM TrinityTM P1（3.0 mm100 mm，3 m）为色谱柱，18 mmol/L乙酸铵（用乙酸调pH 3.4）:乙腈（56:44，:）为淋洗液，在柱温37℃， 流量0.15 mL/min的条件下等度洗脱，电导检测器检测，20 min内完成正丁胺的含量测定。结果表明：正丁胺质量浓度在10.01~500.5 g/mL范围内线性关系良好（r2=0.999 8），检测限为5.05 g/mL（S/N3），定量限为10.01 g/mL（S/N10），日内和日间精密度分为0.33%和0.90%，正丁胺供试品溶液在24 h内稳定（RSD=0.54%），3批正丁胺原料的平均含量为99.79%（RSD=0.125%），3批肿瘤血管抑制剂XY03中正丁胺的平均含量为20.32%（RSD=4.09%），热干燥时，XY03中铵盐的下降率与其溶解度呈正相关。ZTSO技术具有较好的条件优化功能，所建立的方法快速、简便和准确，是正丁胺或含正丁铵盐化合物含量测定的较好方法。
Ion chromatography determination of n-butylamine content based on ZTSO optimization
XIE Hongying1, YONG Zhiquan2, WANG Mengli1, FENG Ya'nan1, SUN Jiayin1, LI Yuqian1, XU Xiaoping1
1. West China School of Pharmacy, Sichuan University, Chengdu 610041, China;
2. Dongguan Daxin Biotech Co., Ltd., Dongguan 523808, China
Abstract: Zhang's technique system organization(ZTSO) has been rapidly optimized and ion chromatography determination of n-butylamine content has been established. AcelaimTM TrinityTM P1 (3.0 mm×100 mm,3 μm) was adopted as chromatographic column. The leacheate was 18 mmol/L ammonium acetate (adjust pH 3.4 by using acetic acid)-acetonitrile(56∶44,ν:ν), and the detector was conductivity detector. Under the condition of 37℃ column temperature and isocratic elution at a flow rate of 0.15 mL/min, the measurement of n-butylamine content could be done in 20 minutes. Show that there was a good linear relationship(r2=0.999 8) at range of the concentration of 10.01-500.5 μg/mL, the limit of detection is 5.05 μg/mL (S/N≥3), the limit of quantization is 10.01 μg/mL(S/N≥10), the intra-day and the inter-day precision were at 0.33% and 0.90% respectively, n-butylamine solution was stable(RSD=0.54%) in 24 hours. The average content of n-butylamine raw materials in three batches are 99.79% (RSD=0.125%), the average n-butylamine content is 20.32% (RSD=4.09%) in three batches of tumor angiogenesis inhibitors XY03. When heat drying, the decrease rate of ammonium salt in XY03 was positively related to its solubility. ZTSO technology has good conditions for optimizing function. The method is rapid, simple and accurate, which is a better method for the assay of n-butylamine or containing the butyl ammonium of compounds.
Keywords: n-butylamine;ion chromatography;content assay;ZTSO
2016, 42(7): 35-38 收稿日期: 2015-12-27;收到修改稿日期: 2016-1-15
基金项目:
作者简介: 谢红英(1991-),女,四川成都市人,硕士研究生,专业方向为药物质量控制。
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