输血用枸橼酸钠注射液3种含量测定方法的比较
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摘要
目的建立和优选输血用枸橼酸钠注射液的含量测定方法。方法 HPLC法采用Waters Symmetry Shield RP18色谱柱(250 mm×4.6 mm,5μm),流动相为0.05 mol·L-1磷酸二氢钾溶液(磷酸调p H2.3)-甲醇(90∶10),检测波长210 nm;离子色谱法采用Ion Pac AS-11-HC离子交换色谱柱(250 mm×4 mm)、AG-11-HC保护柱(50 mm×4 mm),流动相为35 mmol·L-1氢氧化钾溶液,等度洗脱,电导检测器;非水滴定法采用2015年版《中国药典》二部中的方法。结果 HPLC法和离子色谱法中的r分别为0.9999、0.9994,精密度、稳定性、重复性试验的RSD均分别≤1.0%、≤1.5%,平均回收率分别为100.34%、98.16%,RSD分别为0.50%、1.55%(n=9);HPLC法和离子色谱法测定样品的数据与非水滴定法的基本一致,无显著性差异;结论 3种方法均可满足检测要求,但HPLC法的操作更简便、快捷、应用更广泛,最适宜作为输血用枸橼酸钠注射液的含量测定方法。
OBJECTIVE To establish and optimize the determination methods of Sodium citrate injection for transfusion( SCIT).METHODS Column Waters Symmetry Shield RP18(250 mm × 4. 6 mm,5μm) was used with 0. 05 mol·L-1 potassium dihydrogen phosphate solution( adjust with phosphoric acid to a p H 2. 3)-methanol( 90 ∶10) as mobile phase. Detection wavelength was 210 nm. Ion chromatography( IC) used the IC system consisted of a chromatographic column of Ion Pac AS-11-HC(250 mm × 4 mm),and protect column of AG-11-HC(50 mm × 4 mm) and the mobile phase of 35 mmol·L-1 potassium hydroxide solution,isocratic elution,conductive detector. Non-aqueous titration used here was recorded in Chinese Pharmacopoeia( 2015 edition). RESULTS The regression coefficient( r) of HPLC method was 0. 9999. RSD of precision,stability and repeatability experiment were all ≤1. 0%;the average recovery was 100. 34% with the RSD of 0. 50%( n = 9). The r of IC method was 0. 9994,and the RSD of precision,stability and repeatability experiment were all ≤1. 5%,the average recovery was 98. 16%,RSD = 1. 55%( n = 9). The results obtained by HPLC method and IC method basically agree well with Non-aqueous titration method,and they showed no significant difference.CONCLUSION All the three methods meet the detection requirements,but HPLC method is more convenient,faster and more widely used,so it is the most suitable method for the determination of SCIT.
OBJECTIVE To establish and optimize the determination methods of Sodium citrate injection for transfusion( SCIT).METHODS Column Waters Symmetry Shield RP18(250 mm × 4. 6 mm,5μm) was used with 0. 05 mol·L-1 potassium dihydrogen phosphate solution( adjust with phosphoric acid to a p H 2. 3)-methanol( 90 ∶10) as mobile phase. Detection wavelength was 210 nm. Ion chromatography( IC) used the IC system consisted of a chromatographic column of Ion Pac AS-11-HC(250 mm × 4 mm),and protect column of AG-11-HC(50 mm × 4 mm) and the mobile phase of 35 mmol·L-1 potassium hydroxide solution,isocratic elution,conductive detector. Non-aqueous titration used here was recorded in Chinese Pharmacopoeia( 2015 edition). RESULTS The regression coefficient( r) of HPLC method was 0. 9999. RSD of precision,stability and repeatability experiment were all ≤1. 0%;the average recovery was 100. 34% with the RSD of 0. 50%( n = 9). The r of IC method was 0. 9994,and the RSD of precision,stability and repeatability experiment were all ≤1. 5%,the average recovery was 98. 16%,RSD = 1. 55%( n = 9). The results obtained by HPLC method and IC method basically agree well with Non-aqueous titration method,and they showed no significant difference.CONCLUSION All the three methods meet the detection requirements,but HPLC method is more convenient,faster and more widely used,so it is the most suitable method for the determination of SCIT.
引文
[1]樊蓉,张纯,叶朝阳.高浓度枸橼酸钠注射液在血液透析应用的研究进展[J].中国血液净化,2006,5(4):208-211.
[2]中华人民共和国国家药典委员会.中国药典[S].三部.北京:中国医药科技出版社,2015:17.
[3]贾利宁.枸橼酸钠抗凝在血液净化中的应用进展[J].国际移植与血液净化杂志,2006,4(4):7-10.
[4]朱雪妍.离子色谱法测定血栓通注射液中辅料氯化钠和枸橼酸钠的含量[J].药物分析杂志,2015,35(7):1236-1239.
[5]张伟,任连杰,张彤,等.高效阴离子交换色谱法测定人凝血因子Ⅷ中枸橼酸离子的含量[J].中国生物制品学杂志,2014,27(1):125-128.
[6]孔晓锋.非水滴定法应用的注意点[J].乌鲁木齐成人教育学院学报,2003,4:73-74.
[2]中华人民共和国国家药典委员会.中国药典[S].三部.北京:中国医药科技出版社,2015:17.
[3]贾利宁.枸橼酸钠抗凝在血液净化中的应用进展[J].国际移植与血液净化杂志,2006,4(4):7-10.
[4]朱雪妍.离子色谱法测定血栓通注射液中辅料氯化钠和枸橼酸钠的含量[J].药物分析杂志,2015,35(7):1236-1239.
[5]张伟,任连杰,张彤,等.高效阴离子交换色谱法测定人凝血因子Ⅷ中枸橼酸离子的含量[J].中国生物制品学杂志,2014,27(1):125-128.
[6]孔晓锋.非水滴定法应用的注意点[J].乌鲁木齐成人教育学院学报,2003,4:73-74.