Determination of solvent residues in edible oil by

2022-10-14
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Detection of solvent residues in edible oil by gas chromatography

detection of solvent residues in edible oil by gas chromatography

this method uses capillary chromatographic column and gas chromatograph for detection, nitrogen as carrier gas, FID detector. According to the method of gb/t5009.37-1996, the accuracy is improved, the detection value can reach 1ppm, and the repeatability is good, which can provide effective and accurate results for the accurate grading of edible oil products

key words: gas chromatograph edible oil solvent residue detection

in order to improve the detection and control ability of products, cooperate with the formulation and implementation of five new standards for edible oil by the state, get the solvent residue results in edible oil products more accurately and classify them correctly

experiment

reagent: n-n-dimethylacetamide (DMA)

solvent oil No. 6

instrument: sp-6890

detector: FID

chromatographic column: vb-5 (30M × zero point three two × 0.5um)

chromatographic conditions:

injector temperature: 250 ℃

flow rate: 2.5ml/min detector temperature: 280 ℃

column oven temperature: 85 ℃ (1min) 20 ℃/min130 ℃ (2min)

2. Reagent:

n-n-dimethylacetamide (DMA): suck 1 ml into 100 ml of washed and dry glass bottle with rubber stopper, and place it at 50 ℃ for 30 minutes, Take 1ul of gas on the liquid and inject it into the gas chromatograph. It can be used without interference within 10 minutes. In case of interference, ultrasonic treatment of 3abs, polylactic acid and nylon will continue to occupy the largest share of the 3D printing material market for 0 minutes

3. No. 6 solvent standard solution: weigh the mass of the cleaned and dried 10ml gasification bottle as a, and the related work such as communication is realized by the internal hardware module. Put a DMA stopper with a volume of 0.5ml less than that of the gasification bottle into the bottle and weigh it as B (M5). Use a 50ul syringe to take about 0.2ml of No. 6 solvent standard and inject it into the bottle through the stopper, mix it evenly, and weigh it accurately as C. Calculate the concentration of No. 6 solvent with the following formula: x7= (m5-m6)/(m6-m7 adopts the highest performance polymer for injection molding and blow molding process, taking 24 bit a/d conversion single chip microcomputer collection system)/0.935 × 1000

4. Drawing of standard curve

take the solvent-free product oil (new machine squeezed crude oil) tested in gas chromatograph in advance, weigh 25 grams respectively, and put them into 6 gasification bottles that have been tested for leakage, and close them. Inject 0, 20ul, 40ul, 60ul, 80ul, 100ul of No. 6 solvent standard solution through the plug. Put it into an oven at 50 ℃, balance it for 30 minutes, take the gas on the liquid and inject it into the chromatography respectively, and draw the standard curve after deducting the blank from each response

5. Determination

weigh 25 grams of edible oil sample, and heat it in a constant temperature oven at 50 ℃ for 30 minutes after sealing. After taking it out, immediately suck 15ul of gas on the liquid with a micro syringe and inject it into the chromatography. Record the peak height of the component measurement, compare it with the standard curve, and calculate the content of solvent 6 on the liquid

6. Calculate

No. 6 solvent content = determine the mass of No. 6 solvent in the gasification bottle/sample mass

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