PA/PH/OMCL (11) 04 - OMCL Guideline on qualification of HPLC equipment (Annex 1) the reference solution (b) injected after the blank injection.
在对照液（c）中尼泊金丙酯对应的峰面积为空白后进样的对照液（b）中尼泊金丙酯峰面积的0.9-1.1%。
HPLC AUTOSAMPLER 液相色谱仪自动进样器
Thermostatting accuracy and precision can be tested in the frame of the periodic and motivated check of the HPLC Autosampler.
HPLC自动进样器的周期主动检查可以进行温度准确度和精密度检查
THERMOSTATTING ACCURACY 温度准确性 Materials: 材料
Calibrated temperature probe. 校正过的温度探头
Method方法:
Select a temperature along the operational or required temperature range of the equipment. Wait until the system is equilibrated.
在可操作范围或要求的温度范围内选择并设定一个温度，等待系统平衡
By means of the calibrated probe, measure the actual temperature in the autosampler and compare it to the selected temperature.
采用校正过的温度探头，测量自动进样器的实际温度，与设定的温度进行比较
Repeat the same procedure at different pre-selected points covering the temperature range. 在选定的温度范围内不同温度点重复相同的步骤
Limit限度s:
The actual temperature may not differ more than ±3°C with respect to the selected temperature.
实际温度与设定的温度相比差值不超过±3°C
THERMOSTATTING PRECISION 温度准确性
Materials: 材料
Calibrated temperature probe. 校正过的温度探头。
Method方法:
Select a temperature along the operational or required temperature range of the equipment. Wait until the system is equilibrated.
选择一个操作温度或要求的仪器温度范围，等待系统平衡。
By means of the calibrated probe, make ―n‖ measurements over a pre-established period of time. Compare the mean of the ―n‖ measurements to the selected temperature.
采用校正过的温度探头，在预设的时间内进行n次测量，比较n次测量值的平均值与设定的温度。
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PA/PH/OMCL (11) 04 - OMCL Guideline on qualification of HPLC equipment (Annex 1) Limits限度:
The actual temperature may not differ more than ±3°C with respect to the selected temperature.
实际温度与设定的温度之间差值不超过±3°C
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PA/PH/OMCL (11) 04 - OMCL Guideline on qualification of HPLC equipment (Annex 1) HPLC OVEN/COOLING DEVICE 色谱仪柱温箱/降温设施
Thermostatting accuracy is the parameter tested in this example of periodic and motivated check of the HPLC oven/cooling device.
热力学准确性是在本例对HPLC柱温箱/降温设施周期主动检查的参数
THERMOSTATTING ACCURACY 温度准确性
Materials: 材料
Calibrated thermometer. 校正过的温度计
Method方法:
Set the column oven temperature to 40 °C, wait about 30 minutes to equilibrate the system, put a calibrated thermometer into the oven and read the temperature after 10 minutes. 设定柱温箱温度为40 °C，等待约30分钟平衡系统，将校正过的温度计放入柱温箱中，在10分钟后读取温度。
Limits限度: 38 - 42°C.
HPLC UV/DAD DETECTOR 紫外/DAD检测器
The periodic and motivated check of the HPLC UV/DAD detector can be performed by testing the linearity and the wavelength accuracy.
对于HPLC紫外/DAD检测器的周期主动检查，可以对线性和波长准确性进行检查
LINEARITY 线性
Solutions: 溶剂配制
Std. 1: 0.5 μg caffeine/1 ml methanol HPLC Grade 标准2： 0.5 μg咖啡因/1ml色谱级甲醇
Std. 2: 1.0 μg caffeine/1 ml methanol HPLC Grade 标准2： 1.0 μg咖啡因/1ml色谱级甲醇
Std. 3: 5.0 μg caffeine/1 ml methanol HPLC Grade 标准3： 5.0 μg咖啡因/1ml色谱级甲醇
Std. 4: 25.0 μg caffeine/1 ml methanol HPLC Grade 标准4：25.0 μg咖啡因/1ml色谱级甲醇
Std. 5: 50.0 μg caffeine/1 ml methanol HPLC Grade 标准5：50.0 μg咖啡因/1ml色谱级甲醇 Std. 6: methanol HPLC Grade (blank) 标准6：色谱级甲醇（空白）
Std. 5: weigh 9.0 to 11.0 mg caffeine and fill up to 200.0 ml with methanol HPLC 标准5：称取9.0至11.0mg咖啡因，用HPLC级别甲醇稀释至200.0ml Std. 4: dilute 50.0 ml of Std. 5 to 100.0 ml with methanol
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PA/PH/OMCL (11) 04 - OMCL Guideline on qualification of HPLC equipment (Annex 1) 标准4：取50.0ml标准5溶液用甲醇稀释至100.0ml
Std. 3: dilute 10.0 ml of Std. 5 to 100.0 ml with methanol 标准3：取10.0ml标准溶液5用甲醇稀释至100.0ml
Std. 2: dilute 20.0 ml of Std. 3 to 100.0 ml with methanol 标准2：取20.0ml标准3溶液用甲醇稀释至100.0ml
Std. 1: dilute 10.0 ml of Std. 3 to 100.0 ml with methanol 标准1：取10.0ml标准3用甲醇稀释至100.0ml
Settings: 设置
Column: RP-18 5 um 30-50 x 2,1-4.6 mm or capillary 2000 mm x 0.12 mm ID 色谱柱：RP-185 um 30-50 x 2,1-4.6 mm or capillary 2000 mm x 0.12 mm ID Mobile phase: methanol HPLC Grade 流动相：色谱级甲醇 Oven temperature: 40 °C 柱温箱温度：40 °C
Flow rate: 1.0 ml/min (adjusted by using 100% methanol) 流速：1.0ml/min（用100%甲醇调整） Detection: 273 nm 检测波长：273nm Injection volume: 20μl 进样量：20ul
Method方法:
Injection scheme: 进样序列 2 x blank 1 x Std. 1 1 x Std. 2 1 x Std. 3 1 x Std. 4 1 x Std. 5
2针空白，标准1-5依序各一针
Limits限度: r2 ≥ 0.999
Remark: As this test employs different test solutions to be injected, it covers also the check of correct positioning vials in the autosampler.
注：由于此检测中要注入不同溶液，因此也包括了自动进样器样品瓶位置正确性的确认
WAVELENGTH ACCURACY 波长准确度
If there are built-in test procedures for the determination and adjustment of wavelength accuracy, follow the instructions of the instrument manual.
如果内置检测程序可以检测和调节波长准确度，则根据操作手册进行操作 In all other cases use the procedure described below.
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