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含量方法学验证

2011.07.20测

设计量

理论称样量(mg)辅料

80%120100100%150100120%

180100

2011.07.22测

进样重复性考察仪器进样准确性

对照品1022727对照品824602对照品797350对照品716238对照品781518

对照品783324820959.8333105089.919

12.80086

对照品对照品767993762268.25对照品775455777072.5对照品778626776349.5

对照品861997774024.66675458.897540.70526144对照品对照品854403对照品839311对照品862066对照品876155对照品

876585

857983.7515366.11481.79095639

2011.08.05测定2651.53809备注2592.259522621.89880.058699.43052666.056640.05958799.430599.845652677.188230.05983699.84565

100.1347100.13382570.3313

98.899092564.276372567.30380.058699.268922629.030520.060009100.134798.940932629.007810.060008100.1338

100.728399.915482571.53613

99.25962597.151612584.34390.058699.835532613.824460.05926898.8990999.044392623.598880.0594999.26892

98.9622499.33004

2603.52759

2607.990482605.7590.05862636.598880.05929498.940932684.229490.060365100.7283

2556.60889

1.1ml/min,35℃,流动相:1.8%冰乙酸:乙腈(56:44)1.1ml/min,30℃,流动相:1.8%冰乙酸:乙腈(56:44)芬布芬对照品

样品

样品

芬布芬对照品批号:100415-200301,中检所

专属性,耐用性

1.1ml/min,40℃,流动相:1.8%冰乙酸:乙腈(56:44)样品

1.1ml/min,35℃,流动相:1.8%冰乙酸:乙腈(51:49)芬布芬对照品

芬布芬对照品

芬布芬对照品

样品

1.1ml/min,35℃,流动相:1.8%冰乙酸:乙腈(61:39)

2561.414312559.01160.05862614.802250.05987899.915482597.637940.05948599.2596

3183.60913

3186.215333184.91220.05863251.744630.0598399.835533225.976320.05935699.04439

2191.3291

2195.6252193.47710.05862219.915530.05930698.962242228.166020.05952799.330042651.53809

2592.259522621.89880.05862534.010990.05663699.260872543.334470.05684499.62609

2011.08.10测进样重复性

考察仪器进样准确性

rsd%

芬布芬原料

1209734芬布芬原料905734芬布芬原料930590芬布芬原料852126芬布芬原料1049292芬布芬原料1029763

996206.5128676.40912.9166402

2011.08.17测定

称样量(mg)均重(mg)

3034.82593浓度

3032.89746

3029.994383032.57260.059683136.375980.061723103.6582254.25

3131.36670.061624103.4927126.163080.741460.060628102.74793076.571040.060546102.6088125.023133.953130.061675102.4606125.68250.55

3138.146480.061758102.5977125.493069.209720.060401101.6543124.063071.358640.060443101.7254125.693144.976560.061892103.9867253.35

3142.513920.061844103.9052125.663203.860110.063051104.8985126.93160.35986

0.062195

103.4742125.59

1.424254

2011.08.06测定耐用性

样品

芬布芬对照品

样品

1.3ml/min,35℃,流动相:1.8%冰乙酸:乙腈(56:44)芬布芬对照品

样品

0.9ml/min,35℃,流动相:1.8%冰乙酸:乙腈(56:44)芬布芬对照品批号:100415-200301yp110603-1三批中试样品含量yp110601-1yp110601-2yp110602-1yp110602-2芬布芬对照品

yp110603-2

均值sd rsd% 99.5520840.5543740.556868

平均含量%平行样差批平均含量

103.57544

102.678390.89706103.1269 102.5292

101.689840.839354102.1095 103.94595

104.186350.240406104.0662