Determination method of amount of phthalic acid esters
A technology for the determination of phthalic acid and its determination method, which is applied in the field of determination of the total amount of phthalates, can solve problems such as difficult detection of phthalates and complex metabolite components, and achieve sensitivity High, simple operation, good stability
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[0038] Example 1 Determination of the total amount of phthalic acid substances in oil samples
[0039] (1) Prepare standard solutions with phthalic acid concentration of 0.05, 0.1, 1, 10, 25, 50, 100 mg / L with phthalic acid standard stock solution. Separately draw 10μL of the standard solution of each concentration and inject it into the high performance liquid chromatography for analysis. From the high performance liquid chromatography peak area obtained from the corresponding concentration, the standard curve of the peak area-mass concentration of the phthalic acid standard substance and the linear regression equation Y=63331X+ 47465, R 2 =0.9995, and the lowest detection limit is 0.02mg / L.
[0040] (2) After mixing the sample, weigh 2.0g, put it in a reflux bottle, add 10ml of methanol to mix, then add 10ml of KOH solution with a concentration of 2mol / L, reflux in a water bath at 85℃ for 2.5h, and finally remove the device , The methanol is evaporated to dryness in a water bath...
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[0058] Example 2 Determination of the total amount of phthalic acid substances in urine
[0059] (1) Prepare standard solutions with phthalic acid concentration of 0.05, 0.1, 1, 10, 25, 50, 100 mg / L with phthalic acid standard stock solution. Separately draw 10μL of the standard solution of each concentration and inject it into the high performance liquid chromatograph for analysis, and obtain the standard curve of phthalic acid standard substance peak area-mass concentration and linear regression equation Y=63331X+47465, R 2 =0.9995, and the lowest detection limit is 0.02mg / L.
[0060] (2) Take a urine sample by centrifugation at 12000rpm / min for 20min to take the supernatant, take 1ml, add 15μL β-glucuronide hydrolase, and shake at 37°C for 12h.
[0061] (3) The enzymatic hydrolysate was inactivated in boiling water at 100°C. After cooling, centrifuged at 12000rpm / min for 20min to take the supernatant, put it in a reflux bottle, add 10ml of methanol to mix, and then add 15ml of KOH...
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