CN101792383B - Method for extracting low concentration perfluorooctanoic acid from fatty substances - Google Patents
Method for extracting low concentration perfluorooctanoic acid from fatty substances Download PDFInfo
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- CN101792383B CN101792383B CN2010101228799A CN201010122879A CN101792383B CN 101792383 B CN101792383 B CN 101792383B CN 2010101228799 A CN2010101228799 A CN 2010101228799A CN 201010122879 A CN201010122879 A CN 201010122879A CN 101792383 B CN101792383 B CN 101792383B
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Abstract
The invention discloses a method for extracting low concentration perfluorooctanoic acid from fatty substances, comprising the following steps: 1) adding 0.5-2.0g of solid fats or 1.0-3.0ml of liquid fats and normal hexane with mass being 20-50 times that of the solid fats or with volume being 20-50 times that of the liquid fats into a separating funnel and shaking the separating funnel for 5-10min to ensure the fats or oil is dissolved in the normal hexane; 2) adding secondary distilled water with volume being 0.6-1 times that of the normal hexane into the separating funnel and shaking the separating funnel for 10-15min; 3) standing for 16-24h, then discharging the lower aqueous phase into a centrifuge tube, centrifuging the aqueous phase for 10min under 10000r/min and 4 DEG C if the aqueous phase contains insoluble impurities and transferring the supernatant to another centrifuge tube to obtain extract; and 4) using a solid phase extraction device and an HLB column to concentrate and purify the extract to obtain the perfluorooctanoic acid solution. The method is simple in operation, high in extraction efficiency, good in recycling effect and complete in extraction, and the obtained extract is pure, thus reducing damage to the detecting instruments.
Description
Technical field
The present invention relates to a kind of method of from oil substances, extracting the lower concentration Perfluorocaprylic Acid.
Background technology
Perfluorocaprylic Acid (perfluorooctanoic acid); Be called for short PFOA; It is one of perfluorochemical that contains eight carbon atoms; It is applied in the middle of the production of multiple fluoropolymer as the production auxiliary agent, and these polymkeric substance are widely used as textiles, paper, leather, material of construction, the production material of products such as electronic product and non-stick pan and snack food product wrapping material coating.But toxicologic study in recent years proves; PFOA has potential influences embryo growth and development and the risk that possibly cause multiple cancers such as mammary cancer, carcinoma of testis, pancreas tumor and liver tumor; Therefore, a lot of in the world countries with organize production and the use of forbidding this type of material in succession.However; Some researchs show; Comprise in the packing bags such as some fast foods and microwave popcorn still having detected PFOA, and migrate into possibly in picture butter and plant wet goods oil substances or the food, thereby cause the pollution of food oils that health of human body is threatened.Though existing at present PFOA may be moved to the report in the oil substances, and PFOA that from high grease solid matter and liquid edible oil, extracts lower concentration and the report that purifies are not arranged yet.
Migrate into the research of situation in the oil substances for ease of PFOA in the wrapping material that contain anti-oil coating; The present invention is after with the oil substances n-hexane dissolution; With water extraction Perfluorocaprylic Acid wherein; And used the advanced method of the HLB pillar of solid-phase extraction device cooperation Waters company production to sample concentration purification pre-treatment, be intended to inquire into and extract and purify lower concentration Perfluorocaprylic Acid in high oils solid matter and the liquid edible oil.，
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, the method for from oil substances, extracting the lower concentration Perfluorocaprylic Acid that a kind of technology is simple, the recovery is high is provided.
The present invention is for reaching above purpose, and concrete experimental procedure is following:
The method of from oil substances, extracting the lower concentration Perfluorocaprylic Acid comprises the steps:
1) normal hexane with solid grease 0.5～2.0g or liquid oil 1.0～3.0ml and 20～30 times of solid grease quality or liquid oil volume adds in the separating funnel, and concussion 5～10min is dissolved in the middle of the normal hexane grease or oil;
2) redistilled water with 0.6～1 times of normal hexane volume adds in the separating funnel, concussion 10～15min;
3) emit lower floor's water to centrifuge tube after leaving standstill 16～24h, if aqueous phase contains insoluble impurities, then at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution is carried out thickening-purification technology handle, obtain Perfluorocaprylic Acid solution.
Said use solid-phase extraction device carries out the thickening-purification technology treatment step to extracting solution and comprises with addition of the HLB pillar:
1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.0～5.0ml methyl alcohol and 4.0～5.0ml zero(ppm) water;
2) extracting solution passes through the HLB pillar with 1 droplet/second speed;
3) methanol solution with 4.0～5.0ml 20～40% washs the HLB pillars with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4) 4.0～6.0ml methyl alcohol obtains Perfluorocaprylic Acid solution with 1 droplet/second speed wash-out HLB pillar.
The present invention is simple to operate; Extraction efficiency is high, and recovering effect is good, extracts fully; The extracting solution that obtains is pure; Reduced infringement,, can be used for by the extraction of polluted solid oil lipid of lower concentration Perfluorocaprylic Acid and liquid oil Perfluorocaprylic Acid for ensuing accurate detection provides guarantee to detecting instrument.
Embodiment
Embodiment 1
1) 0.5g has been added in the commercially available butter and 15ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 5min is dissolved in the middle of the normal hexane grease;
2) the 15ml redistilled water is added in the separating funnel concussion 10min;
3) emit lower floor's water to centrifuge tube after leaving standstill 16h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.0ml methyl alcohol and 4.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.0ml20% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 4.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 88.4%.
HPLC-MS/MS is the advanced and accurate method of ten minutes that detects at present both at home and abroad Perfluorocaprylic Acid, and wherein extraction recovery is in extracting sample, to add quantitative Perfluorocaprylic Acid and extracting solution is detected the back calculate on the basis of its recovering state and draw.
Embodiment 2
1) 2.0g has been added in the commercially available cream and 30ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 10min is dissolved in the middle of the normal hexane grease;
2) the 30ml redistilled water is added in the separating funnel concussion 15min;
3) emit lower floor's water to centrifuge tube after leaving standstill 24h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 5.0ml methyl alcohol and 5.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 5.0ml30% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 6.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 94.5%.
Embodiment 3
1) 1.0g has been added in the commercially available chocolate and 25ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 8min is dissolved in the middle of the normal hexane grease;
2) the 25ml redistilled water is added in the separating funnel concussion 15min;
3) emit lower floor's water to centrifuge tube after leaving standstill 18h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.5ml methyl alcohol and 4.5ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.5ml40% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 4.5ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 89.1%.
Embodiment 4
1) 1.5g has been added in the commercially available cheese and 75ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 10min is dissolved in the middle of the normal hexane grease;
2) the 30ml redistilled water is added in the separating funnel concussion 15min;
3) emit lower floor's water to centrifuge tube after leaving standstill 24h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.0ml methyl alcohol and 4.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.0ml40% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 4.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 86.6%.
Embodiment 5
1) 2.0ml has been added in the commercially available VT 18 and 30ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 5min is dissolved in the middle of the normal hexane VT 18;
2) the 30ml redistilled water is added in the separating funnel concussion 10min;
3) emit lower floor's water to centrifuge tube after leaving standstill 16h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.0ml methyl alcohol and 4.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.0ml40% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 4.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 93.3%.
Embodiment 6
1) 3.0ml has been added in the commercially available sweet oil and 50ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 10min is dissolved in the middle of the normal hexane sweet oil;
2) the 50ml redistilled water is added in the separating funnel concussion 15min;
3) emit lower floor's water to centrifuge tube after leaving standstill 18h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 5.0ml methyl alcohol and 5.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.0ml40% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 5.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 79.6%.
Embodiment 7
1) 3.0ml has been added in the commercially available peanut oil and 60ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 15min is dissolved in the middle of the normal hexane peanut oil;
2) the 60ml redistilled water is added in the separating funnel concussion 15min;
3) emit lower floor's water to centrifuge tube after leaving standstill 24h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 5.0ml methyl alcohol and 5.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.0ml20% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 5.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 91.4%.
Embodiment 8
1) 2.0ml has been added in the commercially available sunflower seed oil and 40ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 8min is dissolved in the middle of the normal hexane sunflower seed oil;
2) the 30ml redistilled water is added in the separating funnel concussion 12min;
3) emit lower floor's water to centrifuge tube after leaving standstill 20h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.5ml methyl alcohol and 4.5ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 5.0ml20% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 6.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 76.8%.
Embodiment 9
1) 1.5ml has been added in the commercially available rapeseed oil and 50ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 10min is dissolved in the middle of the normal hexane rapeseed oil;
2) the 50ml redistilled water is added in the separating funnel concussion 12min;
3) emit lower floor's water to centrifuge tube after leaving standstill 24h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.0ml methyl alcohol and 4.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.0ml20% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 4.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar; Obtain Perfluorocaprylic Acid solution. also to 2.0ml, use 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 80.7%.
Embodiment 10
1) 1.0ml has been added in the commercially available Oleum Gossypii semen and 30ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 7min is dissolved in the middle of the normal hexane Oleum Gossypii semen;
2) the 20ml redistilled water is added in the separating funnel concussion 15min;
3) emit lower floor's water to centrifuge tube after leaving standstill 16h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.0ml methyl alcohol and 4.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.0ml20% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 4.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 93.7%.
Embodiment 11
1) 1.5ml has been added in the commercially available Semen Maydis oil and 30ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 12min is dissolved in the middle of the normal hexane Semen Maydis oil;
2) the 30ml redistilled water is added in the separating funnel concussion 10min;
3) emit lower floor's water to centrifuge tube after leaving standstill 18h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.0ml methyl alcohol and 4.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.0ml20% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 4.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar; Obtain Perfluorocaprylic Acid solution. also to 2.0ml, use 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 91.1%.
Embodiment 12
1) 1.0ml has been added in the commercially available liquid plam oil and 30ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 10min is dissolved in the middle of the normal hexane liquid plam oil;
2) the 20ml redistilled water is added in the separating funnel concussion 10min;
3) emit lower floor's water to centrifuge tube after leaving standstill 24h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.0ml methyl alcohol and 4.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.0ml25% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 4.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 80.6%.
Embodiment 13
1) 1.0ml has been added in the commercially available til and 20ml normal hexane adding separating funnel of quantitative Perfluorocaprylic Acid, concussion 5min is dissolved in the middle of the normal hexane til;
2) the 20ml redistilled water is added in the separating funnel concussion 10min;
3) emit lower floor's water to centrifuge tube after leaving standstill 16h, at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution carried out thickening-purification technology handle:
4.1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.0ml methyl alcohol and 4.0ml zero(ppm) water;
4.2) extracting solution with 1 droplet/second speed through the HLB pillar;
4.3) wash the HLB pillars with the methanol solution of 4.0ml20% with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4.4) with 4.0ml methyl alcohol with 1 droplet/second speed wash-out HLB pillar, obtain Perfluorocaprylic Acid solution.And use to the 2.0ml 0.22 μ m nylon leaching film to be filtered in the Vestolen PP 7052 bayonet socket sample introduction bottle with the superpure nitrogen air-blowing, using HPLC-MS/MS Detection and Extraction recovery result is 84.3%.
Claims (4)
1. a method of from oil substances, extracting the lower concentration Perfluorocaprylic Acid is characterized in that comprising the steps:
1) normal hexane with solid grease 0.5～2.0g or liquid oil 1.0～3.0ml and 20～50 times of solid grease quality or liquid oil volume adds in the separating funnel, and concussion 5～10min is dissolved in the middle of the normal hexane grease or oil;
2) redistilled water with 0.6～1 times of normal hexane volume adds in the separating funnel, concussion 10～15min;
3) emit lower floor's water to centrifuge tube after leaving standstill 16～24h, if aqueous phase contains insoluble impurities, then at 10000 rev/mins, centrifugal 10min under 4 ℃ of conditions, and supernatant is transferred in another centrifuge tube, obtain extracting solution;
4) use solid-phase extraction device with addition of the HLB pillar, extracting solution is carried out thickening-purification technology handle, obtain Perfluorocaprylic Acid solution.
2. a kind of method of from oil substances, extracting the lower concentration Perfluorocaprylic Acid according to claim 1 is characterized in that said use solid-phase extraction device with addition of the HLB pillar, carries out the thickening-purification technology treatment step to extracting solution and comprises:
1) successively with 2 droplets/second speed the HLB pillar is carried out activation treatment with 4.0～5.0ml methyl alcohol and 4.0～5.0ml zero(ppm) water;
2) extracting solution passes through the HLB pillar with 1 droplet/second speed;
3) methanol solution with 4.0～5.0ml 20～40% washs the HLB pillars with 2 droplets/second, with 2000 rev/mins the HLB pillar is dried;
4) 4.0～6.0ml methyl alcohol obtains Perfluorocaprylic Acid solution with 1 droplet/second speed wash-out HLB pillar.
3. a kind of method of from oil substances, extracting the lower concentration Perfluorocaprylic Acid according to claim 1 is characterized in that said solid grease is cream, cheese, butter or chocolate.
4. a kind of method of from oil substances, extracting the lower concentration Perfluorocaprylic Acid according to claim 1 is characterized in that said liquid oil is VT 18, sweet oil, liquid plam oil, Semen Maydis oil, rapeseed oil, peanut oil, til, sunflower seed oil or Oleum Gossypii semen.
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| CN101450922A (en) * | 2008-12-29 | 2009-06-10 | 浙江大学 | Method for extracting perfluoroetane sulfonic acid and perfluorooctanoic acid ammonium from perfluorochemical-containing solid |
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| CN101450922A (en) * | 2008-12-29 | 2009-06-10 | 浙江大学 | Method for extracting perfluoroetane sulfonic acid and perfluorooctanoic acid ammonium from perfluorochemical-containing solid |
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| Title |
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| Gang LV et al..Determination of Perfluorinated Compounds in Packaging Materials and Textiles Using Pressurized Liquid Extraction with Gas Chromatography–Mass Spectrometry.《ANALYTICAL SCIENCES》.2009,第25卷425-429. * |
| JP特开2003-160531A 2003.06.03 |
| S.P.J. van Leeuwen et al..Extraction and clean-up strategies for the analysis of poly- and perfluoroalkyl substances in environmental and human matrices.《Journal of Chromatography A》.2007,第1153卷172–185. * |
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