建立了高效液相色谱分析方法用来测定药品中乙二醇二乙醚二胺四乙酸（ EGTA）含量，通过检测EGTA与Cu2＋的配合物EGTA?Cu来检测EGTA。采用Ultimate?AQ C18色谱柱（250 mm×4?6 mm，5μm），流动相为乙腈?四丁基氢氧化铵水溶液（质量分数约0?3％四丁基氢氧化铵水溶液，醋酸调pH 6?50）?醋酸钠溶液（35 mmol／L醋酸钠，醋酸调pH 6?50）（20∶20∶60， v／v／v），检测波长为245 nm，流速为1?50 mL／min，柱温为40℃，进样量为100μL。结果表明，EGTA质量浓度在0?10～15?00 mg／L范围内线性关系良好（ R＝0?9998）；以信噪比（ S／N）为3及10确定检出限和定量限，分别为0?05 mg／L 和0?17 mg／L；样品加标平均回收率为98?34％～99?03％， RSD 为1?08％～3?33％（ n＝9）。该方法操作简便，具有分离度好、灵敏度高、重复性好、回收率高等特点，适合药品中EGTA含量的检测，为EGTA检测提供了一种有效的检测方法。
A method was developed for the determination of ethylene glycol bis(2?aminoethyl) ether?N,N,N,N?tetraacetic acid ( EGTA) by high performance liquid chromatography ( HPLC) . The content of EGTA can be determined by that of EGTA?Cu through the complexation between EGTA and Cu2+. The chromatographic separation was performed on an Ultimate?AQ C18 analyti?cal column (250 mm×4?6 mm, 5 μm) using the mobile phase of acetonitrile?ion?pairing rea?gents ( with 0?3% tetrabutyl ammonium hydroxide in mass fraction adjusted to pH 6?50 using acetate)?buffered saline ( 35 mmol/L sodium acetate of pH 6?50 ) ( 20∶20∶60, v/v/v ) . The chromatographic conditions were as follows: flow rate, 1?50 mL/min; detection wavelength, 245 nm;injection volume, 100μL;column temperature, 40℃. Under the conditions, good lin?ear relationships between the mass concentration and the peak area of EGTA were observed in the range of 0?10-15?00 mg/L ( R=0?999 8) . The limit of detection ( LOD, S/N=3) and limit of quantitation (LOQ, S/N=10) were determined as 0?05 mg/L and 0?17 mg/L, respectively. The average recoveries were 98?34%-99?03% with the RSDs of 1?08%-3?33% ( n=9 ) . The results showed that the developed method is sensitive, accurate, reproducible and suitable for the analysis of EGTA in medicine.
参考文献
| [1] | Holroyd C;Kistner U;Annaert W.[J].Molecular Biology of the Cell,199910:3035. |
| [2] | Lovik G;Larsen Sand K;Iversen J G.[J].Scand J Immu-nol,200153:410. |
| [3] | Dominguez K;Ward W S.[J].Syst Biol Reprod Med,200955(5/6):193. |
| [4] | 李恒;晏菊姣;黄京芳.离子色谱法测定氨甲环酸注射液中依地酸二钠的含量[J].药物分析杂志,2012(9):1683-1685. |
| [5] | 韩继永;张秋香;袁玉;陈祥峰.反相高效液相色谱法测定注射用奥美拉唑钠中乙二胺四乙酸二钠含量[J].医药导报,2010(11):1493-1495. |
| [6] | 陆滢.反相高效液相色谱法测定替硝唑氯化钠注射液中乙二胺四乙酸二钠含量[J].中国药业,2013(24):37-38. |
| [7] | 胡巢凤;王彦平;王华东;李楚杰.α-MSH对EGTA发热的作用[J].中国病理生理杂志,1999(4):299-301. |
| [8] | 闫月琴.EGTA-EDTA配位滴定法测定镁钙质耐火材料中的钙和镁[J].建材技术与应用,2002(01):32-33. |
| [9] | 刘兴沂;徐立亚;金玉清.[J].莱钢科技,2011(05):70. |
| [10] | 刘兴沂;徐立亚;魏燕;闫新姝;尹静静.EGTA滴定法直接快速测定硅钙合金中钙[J].莱钢科技,2009(1):78-79. |
| [11] | 王静文;黄湘鹭;曹进;王钢力;张庆生;丁丽霞.超高效液相色谱法同时测定减肥类保健食品中非法添加的25种药物[J].色谱,2014(2):151-156. |
| [12] | 王连珠;周昱;陈泳;王瑞龙;林子旭;林德娟;郑少惠.QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估[J].色谱,2012(2):146-153. |
| [13] | 薛琦;杨龙华.反相离子对高效液相色谱法测定混悬滴眼液中乙二胺四乙酸二钠含量[J].中国药业,2012(1):24-25. |
| [14] | 中华人民共和国药典, 一部[S].北京：中国医药科技出版社,2010. |
| [15] | 罗 R C;郑俊民,.药用辅料手册[M].北京：化学工业出版社,2005 |
| [16] | GB 2760-2011.GB 2760-2011[S]. |
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