HPLC-CAD法同时测定硫酸卡那霉素注射液中卡那霉素和卡那霉素B的含量
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摘要
目的:建立HPLC-CAD法测定硫酸卡那霉素注射液中卡那霉素和卡那霉素B含量的方法。方法:采用Boston Green ODS C18(250 mm×4.6 mm,5μm)色谱柱,以0.2 mol·L~(-1)三氟醋酸溶液-甲醇(95∶5)作为流动相,流速:1.0 ml·min~(-1),柱温:30℃,喷雾温度:55℃,喷雾压力:56.4 psi。结果:卡那霉素在0.385~38.500μg·ml~(-1)之间呈现良好的线性关系(r=0.999 9),检出限为0.075μg·ml~(-1),定量限为0.154μg·ml~(-1),回收率为100.97%(n=9)。卡那霉素B在0.374~37.400μg·ml~(-1)之间呈现良好的线性关系(r=1.000 0),检出限为0.075μg·ml~(-1),定量限为0.150μg·ml~(-1),回收率为100.44%(n=9)。结论:建立的HPLC-CAD测定卡那霉素和卡那霉素B含量的方法检出限低,操作简单准确,可以有效控制硫酸卡那霉素注射液的质量。
Objective: To establish an HPLC with charge aerosol detection( HPLC-CAD) method for the determination of kanamycin and kanamycin B in kanamycin sulfate injection. Methods: The samples were injected into a Boston Green ODS C18( 250 mm×4. 6 mm,5 μm) column. The mobile phase was composed of 0. 2 mol·L~(-1) trifluoroacetic acid aqueous solution-methanol( 95 ∶ 5),the flow rate was 1. 0 ml·min~(-1) and the column temperature was maintained at 30 ℃. The nebulization temperature for the CAD was maintained at 55℃ and the gas pressure was 56. 4 psi. Results: The linear range of kanamycin was 0. 385-38. 500 μg · ml~(-1)( r =0. 999 9),and the limit of detection was 0. 075μg·ml~(-1),the limit of quantitation was 0. 154 μg·ml~(-1),and the average recovery of the method was 100. 97%( n = 9). The linear range of kanamycin B was 0. 374-37. 400 μg·ml~(-1)( r=1. 000 0),and the limit of detection was 0. 075μg·ml~(-1),the limit of quantitation was 0. 150 μg·ml~(-1),and the average recovery of the method was 100. 44%( n= 9). Conclusion: The method for the determination of kanamycin and kanamycin B by HPLC-CAD is simple and accurate,the limit of detection is lower than HPLC-ELSD,and the quality of kanamycin sulfate injection can be effectively controlled.
Objective: To establish an HPLC with charge aerosol detection( HPLC-CAD) method for the determination of kanamycin and kanamycin B in kanamycin sulfate injection. Methods: The samples were injected into a Boston Green ODS C18( 250 mm×4. 6 mm,5 μm) column. The mobile phase was composed of 0. 2 mol·L~(-1) trifluoroacetic acid aqueous solution-methanol( 95 ∶ 5),the flow rate was 1. 0 ml·min~(-1) and the column temperature was maintained at 30 ℃. The nebulization temperature for the CAD was maintained at 55℃ and the gas pressure was 56. 4 psi. Results: The linear range of kanamycin was 0. 385-38. 500 μg · ml~(-1)( r =0. 999 9),and the limit of detection was 0. 075μg·ml~(-1),the limit of quantitation was 0. 154 μg·ml~(-1),and the average recovery of the method was 100. 97%( n = 9). The linear range of kanamycin B was 0. 374-37. 400 μg·ml~(-1)( r=1. 000 0),and the limit of detection was 0. 075μg·ml~(-1),the limit of quantitation was 0. 150 μg·ml~(-1),and the average recovery of the method was 100. 44%( n= 9). Conclusion: The method for the determination of kanamycin and kanamycin B by HPLC-CAD is simple and accurate,the limit of detection is lower than HPLC-ELSD,and the quality of kanamycin sulfate injection can be effectively controlled.
引文
1中国药典[S].2015年版.二部1317
2 王金凤,杨化新,朱俐,等.HPLC-NQAD和HPLC-ELSD法测定硫酸卡那霉素注射剂的含量[J].药物分析杂志,2014,34(4):644-648
3 薛晶,崔学文,胡昌勤.HPLC法测定人用皮卡狂犬病疫苗和皮卡佐剂中硫酸卡那霉素的含量[J].药物分析杂志,2011,31(10):1911-1913
4 姜皓然,李祥鹏,玄光善.柱前衍生化HPLC检测硫酸卡那霉素的方法研究[J].海峡药学,2009,21(7):85-89
5 张明媛,常靓,刘长海,等.柱前衍生化高效液相色谱法检测硫酸阿米卡星注射液中卡那霉素含量的改进[J].药学实践杂志,2013,31(5):343-346
6 张凤妹,王建.HPLC-电喷雾检测器测定硫酸阿米卡星中卡那霉素和硫酸盐的含量[J].中国抗生素杂志,2015,40(5):354-358
7 李心怡,蒋运斌,马逾英.电喷雾检测器在药物HPLC分析中的优势及应用进展[J].中国药房,2017,28(15):2152-2156
8 赵璇,李群,刘兴国,等.ELSD和CAD测定多烯磷脂酰胆碱注射液中磷脂酰胆碱含量的方法比较[J].药物分析杂志,2014,34(3):529-533
9 周洁,姜宏,姚静,等.HPLC-UV-CAD同时测定卡前列素氨丁三醇注射液中主要成分含量[J].中国新药杂志,2015,24(1):22-26
10 高维,方平飞,李焕德,等.PLC-CAD法测定盐酸乙胺丁醇片中盐酸乙胺丁醇的含量[J].中南药学,2009,7(5):338-340
2 王金凤,杨化新,朱俐,等.HPLC-NQAD和HPLC-ELSD法测定硫酸卡那霉素注射剂的含量[J].药物分析杂志,2014,34(4):644-648
3 薛晶,崔学文,胡昌勤.HPLC法测定人用皮卡狂犬病疫苗和皮卡佐剂中硫酸卡那霉素的含量[J].药物分析杂志,2011,31(10):1911-1913
4 姜皓然,李祥鹏,玄光善.柱前衍生化HPLC检测硫酸卡那霉素的方法研究[J].海峡药学,2009,21(7):85-89
5 张明媛,常靓,刘长海,等.柱前衍生化高效液相色谱法检测硫酸阿米卡星注射液中卡那霉素含量的改进[J].药学实践杂志,2013,31(5):343-346
6 张凤妹,王建.HPLC-电喷雾检测器测定硫酸阿米卡星中卡那霉素和硫酸盐的含量[J].中国抗生素杂志,2015,40(5):354-358
7 李心怡,蒋运斌,马逾英.电喷雾检测器在药物HPLC分析中的优势及应用进展[J].中国药房,2017,28(15):2152-2156
8 赵璇,李群,刘兴国,等.ELSD和CAD测定多烯磷脂酰胆碱注射液中磷脂酰胆碱含量的方法比较[J].药物分析杂志,2014,34(3):529-533
9 周洁,姜宏,姚静,等.HPLC-UV-CAD同时测定卡前列素氨丁三醇注射液中主要成分含量[J].中国新药杂志,2015,24(1):22-26
10 高维,方平飞,李焕德,等.PLC-CAD法测定盐酸乙胺丁醇片中盐酸乙胺丁醇的含量[J].中南药学,2009,7(5):338-340