色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
11期
1275-1279
,共5页
山广志%宗艳平%王晓%卢静华
山廣誌%宗豔平%王曉%盧靜華
산엄지%종염평%왕효%로정화
离子色谱法%电导检测器%三磷酸腺苷二钠%有关物质%制剂
離子色譜法%電導檢測器%三燐痠腺苷二鈉%有關物質%製劑
리자색보법%전도검측기%삼린산선감이납%유관물질%제제
ion chromatography(IC)%conductivity detector%adenosine disodium triphosphate (ATP-Na2)%related substances%preparation
建立了用于三磷酸腺苷二钠制剂中主成分及有关物质含量测定的离子色谱方法。采用 IonPac AS11-HC 色谱柱，以 KOH 溶液为淋洗液，梯度洗脱，流速为1.0 mL / min，进样10μL，以 Dionex AERS 5004-mm 抑制器的电导检测器检测，三磷酸腺苷二钠（ATP-Na2）的含量按峰面积以外标法计算，二磷酸腺苷二钠（ ADP-Na2）及单磷酸腺苷二钠（AMP-Na2）按加校正因子的主成分自身对照法计算，未知杂质按主成分自身对照法计算。 ATP-Na2、ADP-Na2及 AMP-Na2的线性范围分别为0.000146~1.83 g / L、0.000484~1.51 g / L 及0.000426~0.804 g / L，相关系数分别为0.9997、0.9996及0.9999；对照品溶液在24 h 内的稳定性良好（峰面积 RSD 分别为1.3％、1.4％、2.5％）；ATP-Na2、ADP-Na2、AMP-Na2的方法定量限（S / N =10）分别为1.5 ng、4.8 ng、4.3 ng，检出限（S / N =3）分别为0.58 ng、1.21 ng、1.28 ng；ATP-Na2在3个水平的加样回收率分别为96.50％、96.57％和96.77％。本方法适用于三磷酸腺苷二钠制剂的质量控制。
建立瞭用于三燐痠腺苷二鈉製劑中主成分及有關物質含量測定的離子色譜方法。採用 IonPac AS11-HC 色譜柱，以 KOH 溶液為淋洗液，梯度洗脫，流速為1.0 mL / min，進樣10μL，以 Dionex AERS 5004-mm 抑製器的電導檢測器檢測，三燐痠腺苷二鈉（ATP-Na2）的含量按峰麵積以外標法計算，二燐痠腺苷二鈉（ ADP-Na2）及單燐痠腺苷二鈉（AMP-Na2）按加校正因子的主成分自身對照法計算，未知雜質按主成分自身對照法計算。 ATP-Na2、ADP-Na2及 AMP-Na2的線性範圍分彆為0.000146~1.83 g / L、0.000484~1.51 g / L 及0.000426~0.804 g / L，相關繫數分彆為0.9997、0.9996及0.9999；對照品溶液在24 h 內的穩定性良好（峰麵積 RSD 分彆為1.3％、1.4％、2.5％）；ATP-Na2、ADP-Na2、AMP-Na2的方法定量限（S / N =10）分彆為1.5 ng、4.8 ng、4.3 ng，檢齣限（S / N =3）分彆為0.58 ng、1.21 ng、1.28 ng；ATP-Na2在3箇水平的加樣迴收率分彆為96.50％、96.57％和96.77％。本方法適用于三燐痠腺苷二鈉製劑的質量控製。
건립료용우삼린산선감이납제제중주성분급유관물질함량측정적리자색보방법。채용 IonPac AS11-HC 색보주，이 KOH 용액위림세액，제도세탈，류속위1.0 mL / min，진양10μL，이 Dionex AERS 5004-mm 억제기적전도검측기검측，삼린산선감이납（ATP-Na2）적함량안봉면적이외표법계산，이린산선감이납（ ADP-Na2）급단린산선감이납（AMP-Na2）안가교정인자적주성분자신대조법계산，미지잡질안주성분자신대조법계산。 ATP-Na2、ADP-Na2급 AMP-Na2적선성범위분별위0.000146~1.83 g / L、0.000484~1.51 g / L 급0.000426~0.804 g / L，상관계수분별위0.9997、0.9996급0.9999；대조품용액재24 h 내적은정성량호（봉면적 RSD 분별위1.3％、1.4％、2.5％）；ATP-Na2、ADP-Na2、AMP-Na2적방법정량한（S / N =10）분별위1.5 ng、4.8 ng、4.3 ng，검출한（S / N =3）분별위0.58 ng、1.21 ng、1.28 ng；ATP-Na2재3개수평적가양회수솔분별위96.50％、96.57％화96.77％。본방법괄용우삼린산선감이납제제적질량공제。
A new method was developed for the determination of adenosine disodium triphos-phate( ATP-Na 2 )and its related substances in ATP-Na 2 preparation by ion chromatography (IC). The sample was diluted with ultrapure water and filtrated by 0. 22 μm polyether sulfone filter membrance,and then analyzed by IC directly without any more pretreatment. The analysis was performed on a Dionex IonPac AS11-HC column(250 mm×4 mm)and a guard column Ion-Pac AG11-HC(50 mm×4 mm). A KOH eluent generator cartridge was used for gradient elution at the flow rate of 1. 0 mL / min. The detection was performed by a Dionex suppressed(Dionex AERS 500 4-mm)conductivity detector. The injection volume was 10 μL. The assay was quanti-tatively completed by external standard method and the related substances were calculated with correction factors. The linear ranges of the method for ATP-Na 2 ,adenosine disodium diphos-phate(ADP-Na2 )and adenosine disodium monophosphate( AMP-Na 2 )were 0. 000 146 - 1. 83 g / L(r = 0. 999 7),0. 000 484-1. 51 g / L( r = 0. 999 6)and 0. 000 426- 0. 804 g / L( r = 0. 999 9), respectively. The average recoveries of ATP-Na 2 were 96. 50% ,96. 57% and 96. 77% at three spiked levels. The limits of quantitation( S / N = 10)of ATP-Na 2 ,ADP-Na 2 and AMP-Na 2 were 1. 5 ng,4. 8 ng,4. 3 ng,and the limits of detection(S / N = 3)were 0. 58 ng,1. 21 ng,1. 28 ng, respectively. The results demonstrated that the system has the advantages of high sensitivity, facile automation and simple sample pretreatment. The method is suitable for the quality control of adenosine disodium triphosphate preparations.
