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Determination of Indic anhydride area normalization method

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1. Scope
This procedure is applicable to the determination of indigo anhydride in Libao physicochemical Technology Co., Ltd.
2. Technical requirements
2.1 appearance: gray white powder;
2.2 main content: ≥ 98.0%;
2.3 moisture: ≤ 0.5%.
3. Determination method
3.1 apparatus
HPLC: UV detector
Chromatographic column: C18 250mm × 4.6mm × 5.0um
3.2 chromatographic conditions
Mobile phase: acetonitrile + water = 50:50 (adjusted pH by acetic acid = 4.0);
Flow rate: 1.0ml/min;
Wavelength: 254nm;
Injection volume: 20 μ L;
Column temperature: 30 ℃.
3.2 determination steps
3.2.1 start up, import analysis method and balance instrument.
3.4 determination method
Area normalization method:
(1) Prepared sample
Weigh 0.06g (accurate to 0.0001) of indigo anhydride sample, put it into a 100ml volumetric flask, fix the volume with acetonitrile, shake in the ultrasonic bath for 5 min, and return to room temperature for standby.
(2) Determination
Under the above operating conditions, after the baseline of the instrument is stable, inject samples continuously for several times until the difference of peak area ratio between the two parallel determinations is no more than 0.5%, and then record the test results.
3.5 result calculation
Take the average value based on the percentage of the peak area of indirubic anhydride in the sample solution of 2 needles.
3.6 error control
The difference between the results of the two determinations is not more than 0.5%, and the arithmetic mean value is taken as the determination result.
4. Determination of moisture content
According to the direct electricity method specified in GB / T 6283-2008.
Weigh 0.1-0.5 g sample to the accuracy of 0.001 G.
Take the arithmetic mean of two parallel determination results as the determination result, and the value is expressed to two decimal places. The error limit of two parallel determination results should not exceed 0.02%.
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