Detection method of benzopyrene in microcapsule powder
A technology of microcapsule powder and detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of low extraction efficiency, low measurement accuracy, insufficient extraction, etc., and achieve the effect of improving the extraction rate
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Embodiment 1
[0028] 1. Materials and instruments
[0029]Materials: methanol is LC-MS grade, purchased from Fisher Company of the United States; ethyl acetate and cyclohexane are HPLC grade, purchased from Fisher Company of the United States; benzo(a)pyrene standard substance; chromatographic column, Agilent ZORBAX SB-C18 ( 100mm×2.1mm, 3.5μm); polyunsaturated fatty acid microcapsule ARA and DHA powder, provided by Carbio Bioengineering (Wuhan) Co., Ltd.
[0030] Instruments: Agilent1260 high performance liquid chromatography, purchased from Agilent Corporation of the United States; QTRAP4500 mass spectrometer, purchased from Sciex Corporation of the United States; refrigerated centrifuge, purchased from Sigma Corporation of the United States; nitrogen blowing instrument, purchased from Shanghai Anpu Scientific Instrument Co., Ltd.); The ultrasonic cleaning machine was purchased from Ningbo Xinzhi Co., Ltd.
[0031] 2. Sample pretreatment
[0032] 2.1 Preparation of standard solution
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Embodiment 2
[0051] 1, material and instrument: with embodiment 1.
[0052] 2. Sample pretreatment
[0053] 2.1 Preparation of standard solution: Same as Example 1.
[0054] 2.2 Extraction of samples
[0055] Weigh 1.0 g (accurate to 0.0001 g) of DHA microcapsule powder product in 3 parts each in a 40 mL plastic centrifuge tube, add 100 μL of benzo(a)pyrene standard solution (concentration 7.5 ng / mL) respectively, add 10 mL of n-hexane, vortex Spin for 60 s, sonicate for 5 min, centrifuge at 7000 r / min for 10 min, take the supernatant as the solution to be tested, and protect the sample from light during the whole process.
[0056] 2.3 Sample purification (refrigerated centrifugal purification)
[0057] Blow the sample to be purified to near dryness with nitrogen at 30°C, dilute to 1mL with methanol, put it into a 1mL centrifuge tube, centrifuge at -10°C, 12000r / min for 15min, take the supernatant, and put it into a 1.5mL injection vial , for analysis by liquid chromatography-tandem ma...
Embodiment 3
[0060] 1, material and instrument: with embodiment 1.
[0061] 2. Sample pretreatment
[0062] 2.1 Preparation of standard solution: Same as Example 1.
[0063] 2.2 Extraction of samples
[0064] Weigh each 3 parts of 1.0g sample (accurate to 0.0001g) of DHA microcapsule powder product in a 40mL plastic centrifuge tube, add 100 μL benzo(a)pyrene standard solution (concentration 7.5ng / mL) respectively, add 10mL n-hexane, Vortex for 30 s, sonicate for 10 min, centrifuge at 10,000 r / min for 5 min, take the supernatant as the solution to be tested, and protect the sample from light during the entire process.
[0065] 2.3 Sample purification (refrigerated centrifugal purification)
[0066] Blow the sample to be purified to near dryness with nitrogen at 30°C, dilute to 1mL with methanol, put it into a 1mL centrifuge tube, centrifuge at -10°C, 12000r / min for 20min, take the supernatant, and put it into a 1.5mL injection vial , for analysis by liquid chromatography-tandem mass spe...
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