柱前衍生HPLC法测定干髓糊剂中多聚甲醛的含量 |
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引用本文: | 危雪平,;马金刚,;郭飞燕,;王鹏远,;王晓娟.柱前衍生HPLC法测定干髓糊剂中多聚甲醛的含量[J].中国药房,2014(37):3507-3510. |
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作者姓名: | 危雪平 ;马金刚 ;郭飞燕 ;王鹏远 ;王晓娟 |
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作者单位: | [1]第四军医大学口腔医院药剂科,西安710032; [2]兰州军区联勤部药品仪器检验所,兰州730050 |
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基金项目: | 军队医疗机构制剂标准提高计划资助项目(No.13ZJZ08) |
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摘 要: | 目的:建立测定干髓糊剂中多聚甲醛含量的方法。方法:采用2,4-二硝基苯肼柱前衍生高效液相色谱法。色谱柱为Diamonsil C18(2),流动相为甲醇-水(60∶40,V/V),流速为1.0 ml/min,检测波长为355 nm,柱温为25℃。结果:多聚甲醛(以甲醛计)检测质量浓度线性范围为5.05252.50μg/ml(r=0.999 7);精密度、重复性、稳定性试验的RSD均小于2%;平均加样回收率为99.12%,RSD=1.86%(n=9)。结论:建立的方法专属性强,结果准确可靠,可用于干髓糊剂中多聚甲醛的含量测定。
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关 键 词: | 柱前衍生 高效液相色谱法 2 4-二硝基苯肼 干髓糊剂 多聚甲醛 含量测定 |
Content Determination of Paraformaldehyde in Mummification Pastes by HPLC with Pre-column Derivatization |
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Affiliation: | WEI Xue-ping, MA Jin-gang, GUO Fei-yan, WANG Peng-yuan, WANG Xiao-juan ( 1 .Dept. of Pharmacy, Hospital of Stomatology, Fourth Military Medical University, Xi'an 710032, China; 2.Institute for Drug and Instrument Control, Joint Logistics Department, Lanzhou Military Command, Lanzhou 730050, China) |
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Abstract: | OBJECTIVE: To establish a method for the content determination of paraformaldehyde in mummification pastes. METHODS: HPLC with pre-column 2, 4-dinitrophenylhydrazine derivatization method was adopted. The determination was performed on Diamonsil C18 (2) column with mobile phase consisted of methanol-water (60 : 40, V/F) at the flow rate of 1.0 ml/min. The UV detection wavelength was set at 355 nm and the column temperature was 25℃. RESULTS: The linear range of paraformaldehyde (calculated by formaldehyde) was 5.05-252.50 μg/ml (r=0.999 7). RSDs of precision, reproducibility and stability tests were all lower than 2%. The average recovery was 99.12% (RSD=1.86%, n=9). CONCLUSIONS: The method is specific, accurate and reliable, and it can be used for the content determination of paraformaldehyde in mummification pastes. |
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Keywords: | Pre-column derivatization HPLC 2 4-dinitrophenylhydrazine Mummification pastes Paraformaldehyde Content determination |
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