Sample pretreatment method for detecting limonin kind compound content in orange peel and seed raw material
A technology of limonoids and sample pretreatment, which is applied in the preparation of test samples, etc., can solve the problems of health hazards for operators, complex processing process, large amount of solvent, etc. thorough effect
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Embodiment 1
[0025] Take 100g of orange seeds, dry and crush them to 80 mesh, take 9 parallel samples, each sample is 0.2g (accurate to 0.001g), add 0.5ml of limonin standard solution with a concentration of 100ug / ml to 3 of them , according to the following method for sample pretreatment: the sample was degreased with 3ml petroleum ether at high speed for 2min, then centrifuged at 4000r / min for 10min, the supernatant was sucked away, and then 3ml petroleum ether was added to the sample, and this operation was repeated twice Add 3ml of acetone to the degreased sample, shake it at high speed for 2min, centrifuge at 4000r / min for 10min, collect the supernatant, repeat the extraction 3 times, combine the acetone extract, and dry the acetone extract at 40°C; the acetone extract Add 1ml of dichloromethane to the solution, ultrasonically dissolve, centrifuge at 4000r / min for 5min, collect the supernatant, repeat the dissolution 3 times, combine the dichloromethane solution, and dilute to 10ml for...
Embodiment 2
[0027] Take 500g of orange seed raw material, dry and pulverize to 60 mesh, take 3 samples in parallel, each sample is 0.2g (accurate to 0.001g), first degrease with 3ml of petroleum ether at high speed for 2min, then centrifuge at 4000r / min for 10min, Aspirate the supernatant, then add 3ml of petroleum ether to the sample, repeat this operation twice; add 3ml of acetone to the degreased sample, extract by high-speed shaking for 2min, centrifuge at 4000r / min for 10min, collect the supernatant, and repeat the extraction for 3 times , combine the acetone extract, dry the acetone extract at 40°C; add 1ml of chloroform to the acetone extract, shake it at high speed to dissolve, centrifuge at 4000r / min for 5min, collect the supernatant, repeat the dissolution 3 times, and combine Chloroform solution, and dilute to 10ml, to be tested. As in Example 1, the spectrophotometric detection results were respectively 13.02%, 12.95%, 13.07%, with an average of 13.01%.
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