Sample pretreatment method for detection of organic chlorine in milk and detection method using same
A technology of organochlorine and milk, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to meet the detection requirements, low recovery rate of organochlorine components, inability to meet immediate and rapid detection, etc., and achieve simple and fast recovery rate, the effect of improving efficiency
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no. 1 example
[0018] The first embodiment: a pre-processing method.
[0019] 1. Instruments, consumables and reagents:
[0020] Rotary evaporator: equipped with vacuum system and heating device;
[0021] Nitrogen blower and centrifuge;
[0022] n-hexane-acetone mixture (9:1): mixed n-hexane and acetone at a volume ratio of 9:1;
[0023] Sodium chloride and magnesium sulfate are analytically pure; organic solvents are chromatographically pure, and the experimental water meets the requirements of GB / T 6682 tertiary water;
[0024] Flori diatomite solid phase extraction column: 500mg / 3mL, the activation method is to rinse the Flori diatomite solid phase extraction column with 3mL n-hexane and 3mL n-hexane-acetone mixture (9:1) in sequence.
[0025] 2. Method steps:
[0026] a. Take 10 grams of milk in a 50mL centrifuge tube, add 20ml of acetonitrile, 4g of magnesium sulfate and 1g of sodium chloride, vortex and mix for 1 minute, and centrifuge at 4000 rpm for 5 minutes; then use a dropper ...
no. 2 example
[0031] The second embodiment: a pre-processing method.
[0032] 1. Instruments, consumables and reagents:
[0033] The instruments, consumables and reagents are the same as those described in the first embodiment.
[0034] 2. Method steps:
[0035] a. Take 10 grams of milk in a 50mL centrifuge tube, add 25ml of acetonitrile, 3g of magnesium sulfate and 1.5g of sodium chloride, vortex and mix for 1.5 minutes, centrifuge at 5000 rpm for 4 minutes; then use a dropper Transfer all the organic phase (i.e. the supernatant after centrifugation) to a 250mL rotary evaporating flask, and rotary evaporate to dryness in a water bath at 55°C;
[0036] b. Clean the rotary evaporator flask with 2 ml of acetonitrile, 4 ml of water and 2 ml of acetonitrile in turn, and transfer to a 50 ml centrifuge tube to combine to obtain the cleaning solution;
[0037] c. Add n-hexane equal to the volume of the cleaning solution to the cleaning solution, vortex and mix for 45 seconds, transfer the organ...
no. 3 example
[0040] The third embodiment: a pre-processing method.
[0041] 1. Instruments, consumables and reagents:
[0042] The instruments, consumables and reagents are the same as those described in the first embodiment.
[0043] 2. Method steps:
[0044] a. Take 10 grams of milk in a 50mL centrifuge tube, add 30ml of acetonitrile, 5g of magnesium sulfate and 2g of sodium chloride, vortex and mix for 2 minutes, and centrifuge at 6000 rpm for 8 minutes; then use a dropper Transfer all the organic phase (i.e. the supernatant liquid after centrifugation) to a 250mL rotary evaporating flask, and rotary evaporate to dryness in a water bath at 60°C;
[0045] b. Clean the rotary evaporating flask with 3 ml of acetonitrile, 6 ml of water and 3 ml of acetonitrile in turn, and transfer to a 50 ml centrifuge tube to combine to obtain the cleaning solution;
[0046] c. Add n-hexane equal to the volume of the cleaning solution to the cleaning solution, vortex and mix for 60 seconds, transfer th...
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