KR200313049Y1 - remaining agricultural chemical extraction apparatus in food - Google Patents

remaining agricultural chemical extraction apparatus in food Download PDF

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KR200313049Y1
KR200313049Y1 KR20-2003-0004967U KR20030004967U KR200313049Y1 KR 200313049 Y1 KR200313049 Y1 KR 200313049Y1 KR 20030004967 U KR20030004967 U KR 20030004967U KR 200313049 Y1 KR200313049 Y1 KR 200313049Y1
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funnel
vacuum
filter paper
distilled water
acetonitrile
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KR20-2003-0004967U
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Korean (ko)
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박제원
이석범
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대한민국(국립농산물품질관리원장)
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D33/00Filters with filtering elements which move during the filtering operation
    • B01D33/15Filters with filtering elements which move during the filtering operation with rotary plane filtering surfaces
    • B01D33/17Filters with filtering elements which move during the filtering operation with rotary plane filtering surfaces with rotary filtering tables
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D33/00Filters with filtering elements which move during the filtering operation
    • B01D33/80Accessories
    • B01D33/82Means for pressure distribution
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/02Food
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2201/00Details relating to filtering apparatus
    • B01D2201/20Pressure-related systems for filters
    • B01D2201/204Systems for applying vacuum to filters
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • G01N2001/4061Solvent extraction

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Pathology (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Food Science & Technology (AREA)
  • Molecular Biology (AREA)
  • Biomedical Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

본 고안의 잔류농약 추출장치는 일측에 진공발생장치와 연결되는 진공밸브가 마련되고 타측에 배출밸브가 마련되며 밀폐된 내부공간을 형성하는 진공하우징과, 진공하우징에 회전가능하게 지지되는 턴테이블과, 턴테이블에 원주방향으로 일정간격으로 마련되는 복수의 깔대기와, 각 깔대기에 놓여지는 C18이 함유된 여과지와, 각 깔대기에 아세토니트릴과 증류수를 각각 공급시키는 제1,2공급호스와, 각 깔대기를 함께 연통시키며 그 단부가 진공하우징에 위치되는 연결관을 구비하여서, 진공발생장치에 의한 진공에 의해서 상기 아세토니트릴과 증류수가 감압여과되도록 구성된다.Residual pesticide extraction device of the present invention is provided with a vacuum valve connected to the vacuum generating device on one side, the discharge valve is provided on the other side and the vacuum housing to form a closed inner space, a turntable rotatably supported in the vacuum housing, A plurality of funnels arranged at regular intervals in the circumferential direction on the turntable, filter paper containing C 18 placed in each funnel, first and second supply hoses for supplying acetonitrile and distilled water to each funnel, and each funnel It is provided with a connecting tube in communication with the end thereof and positioned at the vacuum housing, so that the acetonitrile and the distilled water are filtered under reduced pressure by a vacuum generated by the vacuum generator.

본 고안의 잔류농약 추출장치는 유기용매(아세토니트릴)로 농산물 중 잔류된 농약을 추출하고 추출용매에 증류수를 가하여 친수성으로 전환하여 여과지를 통과시켜 잔류농약을 추출함으로써, 우수한 정제효과를 발휘함은 물론 농축과정을 없애 이 과정에서의 분석물질 손실을 줄이고, 분석소요시간을 절약할 수 있다.The residual pesticide extracting apparatus of the present invention extracts the pesticide residue in agricultural products with an organic solvent (acetonitrile), adds distilled water to the extraction solvent, converts it into hydrophilicity, passes the filter paper and extracts the residual pesticide, and shows excellent purification effect. Of course, the concentration process can be eliminated to reduce analyte loss and save analysis time.

Description

식품내 잔류농약 추출장치{remaining agricultural chemical extraction apparatus in food}Residual agricultural chemical extraction apparatus in food

본 고안은 식품내 잔류농약 추출장치에 관한 것으로써, 특히 식품에 함유된 농약을 추출하는데 소요시간을 대폭 단축시킨 식품내 잔류농약 추출장치에 관한 것이다.The present invention relates to an apparatus for extracting residual pesticides in food, and more particularly, to an apparatus for extracting residual pesticides in food, which greatly reduces the time required for extracting pesticides contained in foods.

농산물의 잔류 농약을 분석하는 방법은 GC, GC/MS, LC, LC/MS 등의 분석기기를 이용한 방법이나 효소 등을 이용한 독성 시험법이 있다.Methods of analyzing the residual pesticides of agricultural products include methods using analyzers such as GC, GC / MS, LC, LC / MS, and toxicity tests using enzymes.

통상의 다성분 동시분석방법은 추출, 농축, 정제 등의 전처리 조작 과정을 거친 후 GC, GC/MS 등의 분석기기 시험 조작을 거친다The conventional multi-component simultaneous analysis method undergoes pretreatment operation such as extraction, concentration, and purification, and then undergoes test operation of analyzer such as GC and GC / MS.

첫 번째 단계인 추출과정은 시료를 정밀히 달아 혼합 추출분쇄기병에 넣고 아세토니트릴 100ml를 넣은 후 혼합추출분쇄기로 2 ∼ 3분간 균질화한다. 이를 여지가 깔려 있는 부크너 깔대기로 옮겨 감압(減壓) 여과한다. 여액을 염화나트륨 10∼15g이 들어있는 150ml의 분리병에 담고 마개를 막은 후 1분간 세게 흔들어 섞고, 이를 약 1시간 정치하여 아세토니트릴층과 물층을 분리시킨다.In the first step, the extraction process is precisely weighed, placed in a mixed extractive grinder bottle, 100 ml of acetonitrile, and homogenized for 2 to 3 minutes with a mixed extractive grinder. It is transferred to a Buchner funnel with room for pressure and filtered under reduced pressure. The filtrate is placed in a 150 ml separator containing 10 to 15 g of sodium chloride. The cap is closed, shaken vigorously for 1 minute, and left to stand for about 1 hour to separate the acetonitrile layer and the water layer.

두 번째 단계인 농축과정은 위의 과정에서 분리된 액(아세토니트릴층) 20ml를 50ml의 비이커에 취하여 40℃이하의 수욕조 중에서 공기 또는 질소가스를 통과시키면서 용매가 소량 남을 때까지 증발시키고 다시 20% 아세톤 함유 핵산 2ml를 넣고 시험관 교반기로 벽면의 잔류물을 완전히 녹인다.The second step, the concentration process, takes 20 ml of the liquid (acetonitrile layer) separated in the above process into a 50 ml beaker and evaporates until a small amount of solvent remains while passing air or nitrogen gas in a water bath below 40 ° C. Add 2 ml of% acetone-containing nucleic acid and completely dissolve the residue on the wall with a test tube stirrer.

세 번째 단계인 정제과정은 후로리실(Florisil;500mg) 고정상이 충전되어 있는 일회용 카트리지(용량 2ml)를 사용하여 카트리지에 미리 핵산 5ml를 초당 2∼3방울정도의 속도로 유출하여 버리고, 이 카트리지에 20% 아세톤 함유 핵산 5ml를 위와 같은 방법으로 유출하여 버린다.The third step, the purification process, uses a disposable cartridge (2 ml volume) filled with a Florisil (500 mg) stationary phase and 5 ml of nucleic acid is pre-flowed into the cartridge at a rate of 2-3 drops per second. 5 ml of 20% acetone-containing nucleic acid is spilled in the same manner as above.

이어서 상기 농축과정에서 얻은 잔류물을 녹인 액을 카트리지 상단에 넣고 초당 1∼2방울 정도의 속도로 용출시켜 시험관에 받고 다시 카트리지가 용매에 젖은 상태에서 20% 아세톤 함유 핵산 5ml를 용출하여 동일 시험관에 모으고 내부표준물질을 첨가한다.Subsequently, a solution of the residue obtained in the concentration process was put on the top of the cartridge, eluted at a rate of 1 to 2 drops per second, and received in a test tube. Then, 5 ml of 20% acetone-containing nucleic acid was eluted while the cartridge was wet with a solvent. Collect and add internal standards.

용출액은 40℃이하의 수욕조 중에서 질소 또는 공기를 낮은 유속으로 통과시키면서 용매를 날려보낸 후 20% 아세톤 함유 핵산에 녹여서 일정량으로 하여 시험용액으로 한다.The eluate is blown through the solvent while passing nitrogen or air at a low flow rate in a water bath below 40 ℃, and dissolved in 20% acetone-containing nucleic acid to make a test solution.

이와 같이 농산물 중 잔류농약을 분석하기 위해서는 복잡한 추출과 농축, 정제 등의 전처리방법이 요구되어 많은 시간이 소요될 뿐만 아니라, 숙련된 분석기술자가 필요하여 빠른 시간 내에 농산물의 안전성 여부를 확인하기가 불가능하였다.As such, the analysis of residual pesticides in agricultural products requires a complex pretreatment method such as extraction, concentration, and purification, which takes a lot of time, and requires skilled analytical engineers to confirm the safety of agricultural products in a short time. .

이에 따라서 잔류농약 유무확인 시간이 많이 소요되어 대부분 농산물의 안전성 분석 결과는 소비자가 농산물을 섭취하고 난 후에나 알 수 있다.As a result, it takes a long time to confirm the presence of residual pesticides, and the results of safety analysis of most agricultural products can be known only after the consumers consume the agricultural products.

또한, 농축을 위한 주변분석장비(수욕조, 질소가스발생장치 또는 질소가스봄배 등)가 추가로 소요된다.In addition, peripheral analysis equipment (such as a water bath, nitrogen gas generator or nitrogen gas spring) for concentration is additionally required.

본 고안은 상기와 같은 문제점을 해결하기 위하여 창출된 것으로써, 식품으로부터 잔류농약성분을 신속하게 추출할 수 있게 하여 유통중인 농산물도 신선상태에서 안전성 확인이 가능함은 물론, 수입농산물 검역, 수출농산물의 안전성 확보를 통한 국내농산물의 품질 향상에 기여할 수 있도록 한 식품내 잔류농약 추출장치를 제공하는 데 그 목적이 있다.The present invention has been created to solve the above problems, it is possible to quickly extract the residual pesticide components from food to ensure that the agricultural products in circulation in the fresh state, as well as the inspection of imported agricultural products, export agricultural products The purpose is to provide a device for extracting residual pesticides in food that can contribute to the improvement of the quality of domestic agricultural products through securing safety.

도 1은 종래 잔류농약 추출방법을 나타낸 흐름도,1 is a flow chart showing a conventional residual pesticide extraction method,

도 2 내지 도 4는 본 고안의 잔류 농약 추출장치를 설명하기 위한 개략도이다.2 to 4 is a schematic diagram for explaining the residual pesticide extraction apparatus of the present invention.

* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings

10...진공하우징 20...턴테이블10 ... vacuum housing 20 ... turntable

30...조절밸브 50...용기수용관30 ... control valve 50 ... container vessel

60...깔대기 70...연결튜브60 ... funnel 70 ... connection tube

80...여과지 90...중공컵80 ... paper 90 ... hollow cup

상기 목적을 달성하는 본 고안의 식품내에 함유된 잔류농약 추출장치는 일측에 진공발생장치와 연결되는 진공밸브가 마련되고 타측에 배출밸브가 마련되며 밀폐된 내부공간을 형성하는 진공하우징과,Residual pesticide extraction device contained in the food of the present invention to achieve the above object is provided with a vacuum valve connected to the vacuum generating device on one side and the discharge valve is provided on the other side and the vacuum housing to form a closed inner space,

상기 진공하우징에 회전가능하게 지지되는 턴테이블과,A turntable rotatably supported by the vacuum housing;

상기 턴테이블에 원주방향으로 일정간격으로 마련되는 복수의 깔대기와,A plurality of funnels provided at regular intervals in the circumferential direction on the turntable;

상기 각 깔대기에 놓여지는 C18이 함유된 여과지와,Filter paper containing C 18 placed in each funnel,

상기 각 깔대기에 아세토니트릴과 증류수를 각각 공급시키는 제1,2공급호스와,First and second supply hoses for respectively supplying acetonitrile and distilled water to each funnel;

상기 각 깔대기를 함께 연통시키며 그 단부가 상기 진공하우징에 위치되는 연결관을 구비하여서,Each connecting funnel in communication with an end of which is located in the vacuum housing,

상기 진공발생장치에 의한 진공에 의해서 상기 아세토니트릴과 증류수가 감압 여과되도록 된 것을 특징으로 한다.The acetonitrile and distilled water are filtered under reduced pressure by a vacuum by the vacuum generator.

또한, 본 고안 장치는 상기 각 깔대기 상부에 위치되며 상하단부가 개구된 중공컵과, 상기 깔대기와 중공컵을 연결시키는 연결튜브와, 상기 중공컵과 상기 여과지 사이에 마련되어 밀폐시키는 오링과, 상기 깔대기 상단에 마련되어 상기 여과지를 지지시키는 유리섬유를 구비하여 된 구조를 가진다.In addition, the device of the present invention is located above each funnel, the upper and lower ends of the hollow cup, the connection tube connecting the funnel and the hollow cup, the O-ring provided between the hollow cup and the filter paper and sealed, the top of the funnel It has a structure provided in the glass fiber provided to support the filter paper.

상기 각 깔대기에 대응하는 턴테이블에는 상기 발생된 진공을 개폐하며 상기 연결관과 연결되는 복수의 조절밸브가 마련되고, 상기 각 조절밸브에 연결되는 지지관과, 상기 각 지지관의 상단에 지지되며 상기 깔대기가 지지되는 용기수용관과, 상기 각 용기수용관에 수용되어 상기 여과지로부터 용해되는 잔류농약이 수용되는 용기와, 상기 용기수용관과 깔대기 사이를 밀폐하는 밀폐링을 구비하여 된 구조를 가진다.The turntable corresponding to each funnel is provided with a plurality of control valves that open and close the generated vacuum and are connected to the connection pipes, support tubes connected to the control valves, and supported on the upper ends of the support tubes, And a container containing a funnel holding vessel, a container containing residual pesticides contained in each container receiving tube and dissolved from the filter paper, and a sealing ring for sealing between the container receiving tube and the funnel.

또한, 상기 각 제1,2공급호스는 각각 아세트니트릴 저장조와 증류수 저장조에 연결되고, 상기 각 저장조로부터 아세트니트릴과 증류수가 각각 정량공급모터에 의해서 정량적으로 공급되도록 함이 바람직하다.In addition, each of the first and second supply hoses are connected to the acetonitrile storage tank and the distilled water storage tank, respectively, it is preferable that the acetonitrile and distilled water from each of the storage tank to be quantitatively supplied by the quantitative supply motor.

이하 첨부된 도면을 참조하면서 본 고안에 따른 바람직한 실시예를 상세히 설명한다.Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

본 고안 식품내 잔류농약 추출장치는 분석을 위한 잔류농약의 추출소요시간이 대폭 단축시키고, 추출장비 또한 간단하고 간편하게 사용할 수 있게 한다.Invented residual pesticide extraction device in the food greatly reduces the extraction time of the residual pesticides for analysis, and the extraction equipment can also be used simply and simply.

도 2 내지 도 4에 도시된 바와 같이 본 고안의 잔류 농약 추출장치는 일측에 진공발생장치(미도시)와 연결되는 진공밸브(11)가 마련되고 타측에 배출밸브(12)가 마련되며 밀폐된 내부공간을 형성하는 진공하우징(10)과, 상기 진공하우징(10)에 회전가능하게 지지되는 턴테이블(20)과, 상기 턴테이블(20)에 원주방향으로 일정간격으로 마련되는 복수의 깔대기(60)와, 상기 각 깔대기(60)에 놓여지는 C18이 함유된 여과지(80)와, 상기 각 깔대기(60)에 아세토니트릴과 증류수를 각각 공급시키는 제1,2공급호스(112)(122)와, 상기 각 깔대기(60)를 함께 연통시키며 그 단부가 상기 진공하우징(10)에 위치되는 연결관(21)을 구비한다.As shown in FIGS. 2 to 4, the residual pesticide extracting apparatus of the present invention has a vacuum valve 11 connected to a vacuum generator (not shown) on one side and a discharge valve 12 provided on the other side of the apparatus. A vacuum housing 10 forming an inner space, a turntable 20 rotatably supported by the vacuum housing 10, and a plurality of funnels 60 provided at predetermined intervals in the circumferential direction on the turntable 20. And, filter paper 80 containing C 18 placed in each funnel 60, First and second supply hoses 112, 122 to supply acetonitrile and distilled water to each funnel 60 and In addition, each funnel (60) is communicated with the end portion thereof is provided with a connecting pipe (21) located in the vacuum housing (10).

상기 턴테이블(20)은 베어링(22)에 의해 진공하우징(10)에 대해 회전가능하다.The turntable 20 is rotatable relative to the vacuum housing 10 by means of a bearing 22.

또한, 상기 각 깔대기(60) 상단에는 상하단부가 개구된 중공컵(90)이 얹혀지고, 상기 깔대기(60)와 중공컵(90)은 연결튜브(70)에 의해서 연결되어 있다.In addition, the upper and lower ends of the hollow cup 90 is placed on the top of each funnel 60, the funnel 60 and the hollow cup 90 is connected by a connection tube (70).

상기 중공컵(90)과 상기 여과지(80) 사이에는 밀폐를 위한 오링(81)이 마련되고, 상기 깔대기(60) 상단에는 상기 여과지(80)를 평평하게 지지시키는 유리섬유(82)가 마련되어 있다.An o-ring 81 for sealing is provided between the hollow cup 90 and the filter paper 80, and a glass fiber 82 is provided on the top of the funnel 60 to flatly support the filter paper 80. .

또한, 상기 각 깔대기(60)에 대응하는 턴테이블(20)에는 상기 발생된 진공을 개폐하며 상기 연결관(21)과 연결되는 복수의 조절밸브(30)가 마련되고, 상기 각 조절밸브(30)에는 지지관(40)이 연결되어 있다. 상기 각 지지관(40)의 상단에는 상기 깔대기(60)가 지지되는 용기수용관(50)이 안착되고, 상기 용기수용관(50)과 깔대기(60) 사이에는 밀폐를 위한 밀폐링(51)이 마련되어 있다.In addition, the turntable 20 corresponding to each funnel 60 is provided with a plurality of control valves 30 which open and close the generated vacuum and are connected to the connection pipe 21, and each of the control valves 30. The support pipe 40 is connected. The upper end of each of the support tube 40, the container receiving tube 50 to which the funnel 60 is supported is seated, the sealing ring for sealing between the container receiving tube 50 and the funnel 60 (51) This is provided.

한편, 상기 각 용기수용관(50)에는 상기 여과지(80)로부터 용해되는 잔류농약이 수용되는 용기(130)가 수용된다.On the other hand, each container housing tube 50 is accommodated in the container 130 is accommodated for the residual pesticide dissolved from the filter paper (80).

또한, 상기 각 제1,2공급호스(112)(122)는 각각 아세트니트릴 저장조(110)와 증류수 저장조(120)에 연결되고, 상기 각 저장조(110)(120)로부터 아세트니트릴과 증류수가 각각 정량공급모터(111)(121)에 의해서 상기 각 중공컵(90)에 정량적으로 공급되도록 되어 있다.In addition, each of the first and second supply hoses 112 and 122 is connected to the acetonitrile reservoir 110 and the distilled water reservoir 120, respectively, and the acetonitrile and distilled water from the respective reservoir 110 and 120, respectively. The fixed quantity supply motors 111 and 121 are quantitatively supplied to the respective hollow cups 90.

상기 여과지(80)는 미국(3M사)에서「C18 Empore Extraction Disks」로 제작된 것으로서, 90%±2%의 흡착물질과 10%±2%의 PTFE(polytetrafluoroethylene)으로 만들어진 두께 0.50mm±0.05mm의 얇은 막으로 구성되어 있어 흡착용량이 적어 불순물이 적은 시료분석에 적합하다.The filter paper 80 is made of "C18 Empore Extraction Disks" in the United States (3M company), made of 90% ± 2% of the adsorbent material and 10% ± 2% PTFE (polytetrafluoroethylene) 0.50mm ± 0.05mm It is composed of a thin membrane of which is suitable for sample analysis with less impurities due to low adsorption capacity.

이와 같은 여과지는, 상술한 종래의 카트리지를 사용함에 따라 카트리지내의고정상이 수직방향으로 작용하여 표면적이 적은 카트리지 크기 및 로딩(loading) 시험액량간의 흡착용량 한계로 재현성에 차이가 있었던 것과는 달리, 표면적이 넓은 원형의 형태로 제작 사용됨으로써 재현성 실현에 유리하다.This filter paper has a surface area that is different from the reproducibility due to the limitation of adsorption capacity between the cartridge size and the loading test liquid amount of which the fixed phase in the cartridge acts in the vertical direction by using the above-described conventional cartridge. It is advantageous to realize reproducibility by making and using in a wide circular shape.

본 고안의 잔류 농약의 추출장치의 동작은 다음과 같다.The operation of the extraction device of the residual pesticide of the present invention is as follows.

먼저, 제1공급호스(112)를 통하여 아세토니트릴 10ml를 각각의 중공컵(90)에 공급하여서, 여과지(80)를 통하여 감압여과시킨다. 이때 진공발생장치(미도시)를 통한 진공흡입력은 연결관(21)을 통하여 각 여과지(80)에 공통으로 작용된다.First, 10 ml of acetonitrile is supplied to each of the hollow cups 90 through the first supply hose 112 and filtered under reduced pressure through the filter paper 80. At this time, the vacuum suction input through the vacuum generator (not shown) acts in common to each filter paper 80 through the connecting pipe (21).

각 여과지(80)로부터 아세토니트릴 또는 메탄올이 진공압에 의해서 여과되기 시작하면, 진공발생을 멈추고 자연여과상태에서 여과지(80)가 건조되지 않도록 한다.When acetonitrile or methanol begins to be filtered from each filter paper 80 by vacuum pressure, the vacuum generation is stopped and the filter paper 80 is not dried in a natural filtration state.

이와 같은 상태에서 조절밸브(30)의 조절콕(31)을 잠근 상태에서 제2공급호스(122)를 통하여 각 중공컵(90)에 증류수 220ml를 공급한 후 상기 원심분리된 상등액인 아세토니트릴층 20ml을 혼합시킨다.In this state, 220 ml of distilled water was supplied to each of the hollow cups 90 through the second supply hose 122 while the control cock 31 of the control valve 30 was locked, and the acetonitrile layer as the supernatant was centrifuged. 20 ml are mixed.

이후 조절콕(31)을 오픈하고 진공발생장치를 가동하여 진공도를 20mmHg로 유지시키면서 감압여과시킨다. 이때 농약은 여과지에 흡수하게 되고 불순물들은 여과지를 통하여 배출되게 된다. 즉, 친수성 유기용매를 사용하여 여과지(80)에 통과시키는 조작으로 친수성 방해물질은 여과지(80)를 통과하여 제거된다.Thereafter, the adjusting cock 31 is opened and the vacuum generator is operated to filter the pressure under reduced pressure while maintaining the vacuum degree at 20 mmHg. At this time, the pesticide is absorbed in the filter paper and impurities are discharged through the filter paper. That is, the hydrophilic interference substance is removed through the filter paper 80 by the operation of passing the filter paper 80 using a hydrophilic organic solvent.

이와 같이 제거된 방해물질들은 진공하우징(10)의 배출밸브(12)를 통하여 배출되게 된다.The obstacles thus removed are discharged through the discharge valve 12 of the vacuum housing 10.

여과가 종료되면 여과지(80)를 분리하여 중공컵(90) 및 깔대기(60) 주변을 아세톤(acetone)으로 세정하고, 도 2에 도시된 바와 같이 깔대기(60) 하부에 용기(130)를 위치시키고 다시 여과지(80)를 장착해 20% 아세톤(acetone)이 포함된 핵산(n-Hexane) 4ml를 여과지(80)에 공급한다. 이때 여과지(80)에 흡수된 농약이 용출된다. 여과지로부터 용출되는 잔류농약은 시료용기(130)에 수용된다. 농약 분석시에는 용출액에 적당량의 무수황산나트륨을 가해 탈수시켜 기기분석을 수행한다.When the filtration is finished, the filter paper 80 is separated to wash the hollow cup 90 and the funnel 60 around with acetone, and the container 130 is positioned below the funnel 60 as shown in FIG. 2. Then, the filter paper 80 is mounted again, and 4 ml of nucleic acid (n-Hexane) containing 20% acetone is supplied to the filter paper 80. At this time, the pesticide absorbed by the filter paper 80 is eluted. Residual pesticide eluted from the filter paper is accommodated in the sample container (130). In the analysis of pesticides, an appropriate amount of anhydrous sodium sulfate is added to the eluate and dehydrated.

상기에 있어서, 각 중공컵(90)에 공급되는 아세토니트릴 및 증류수는 정량공급모터(111)(121)에 의해서 정량적으로 공급이 가능하며, 턴테이블(20)의 회전으로 각 중공컵(90)에의 공급이 간편하다.In the above, acetonitrile and distilled water supplied to each hollow cup 90 can be quantitatively supplied by the fixed-quantity supply motors 111 and 121, and the rotation of the turntable 20 to each hollow cup 90. Supply is simple.

상기 추출장치에는 정량공급모터 및 전원공급등을 제어하기 위한 제어판(미도시)이 설치되고, 진공하우징(10)에는 폐용매 유량확인용 게이지(미도시) 설치된다.The extraction apparatus is provided with a control panel (not shown) for controlling a fixed-quantity supply motor and power supply, and the vacuum housing 10 is provided with a waste solvent flow rate check gauge (not shown).

상술한 바와 같은 본 고안은 다음과 같은 이점을 가진다.The present invention as described above has the following advantages.

첫째, 유기용매(아세토니트릴)로 농산물 중 잔류된 농약을 추출하고 추출용매에 증류수를 가하여 친수성으로 전환하여 여과지를 통과시켜 잔류농약을 추출함으로써, 우수한 정제효과를 발휘함은 물론 농축과정을 없애 이 과정에서의 분석물질 손실을 줄이고, 분석소요시간을 절약할 수 있다.First, extract residual pesticides from agricultural products with organic solvent (acetonitrile), add distilled water to extraction solvent, convert to hydrophilicity and pass filter paper to extract residual pesticides. It can reduce analyte loss in the process and save analysis time.

둘째, 분석 절차가 간단하여 주변 분석장비의 설치비용 및 설치공간을 대폭경감시키고, 수입농산물의 신속한 통관을 가능하게 한다.Second, the analysis process is simple, which greatly reduces the installation cost and installation space of the surrounding analysis equipment, and enables the rapid customs clearance of imported agricultural products.

셋째, 분석소요 시약 사용량이 적어 친환경적인 분석이 가능하다.Third, it is possible to use eco-friendly analysis because the amount of reagent required for analysis is small.

넷째, 종래 복잡한 추출과 농축, 정제 등의 전처리방법이 요구되어 많은 시간이 소요될 뿐만 아니라 숙련된 분석기술자가 필요하였던 것과는 달리, 전문인력의 절감이 가능하다Fourth, the conventional complex extraction, concentration, and pre-treatment methods such as purification is required not only takes a lot of time, but also requires a skilled analysis engineer, it is possible to reduce the professional manpower

다섯째, 분석과정에서 추출액 농축시 산화/휘산에 의한 목적물의 손실을 줄일 수 있다.Fifth, it is possible to reduce the loss of the target by the oxidation / volatilization during the concentration of the extract during the analysis.

Claims (4)

식품내 잔류농약을 추출하기 위한 장치에 있어서,In the device for extracting residual pesticides in food, 일측에 진공발생장치와 연결되는 진공밸브가 마련되고 타측에 배출밸브가 마련되며 밀폐된 내부공간을 형성하는 진공하우징과,A vacuum housing connected to a vacuum generating device on one side and a discharge valve on the other side, and a vacuum housing forming an enclosed inner space; 상기 진공하우징에 회전가능하게 지지되는 턴테이블과,A turntable rotatably supported by the vacuum housing; 상기 턴테이블에 원주방향으로 일정간격으로 마련되는 복수의 깔대기와,A plurality of funnels provided at regular intervals in the circumferential direction on the turntable; 상기 각 깔대기에 놓여지는 C18이 함유된 여과지와,Filter paper containing C 18 placed in each funnel, 상기 각 깔대기에 아세토니트릴과 증류수를 각각 공급시키는 제1,2공급호스와,First and second supply hoses for respectively supplying acetonitrile and distilled water to each funnel; 상기 각 깔대기를 함께 연통시키며 그 단부가 상기 진공하우징에 위치되는 연결관을 구비하여서,Each connecting funnel in communication with an end of which is located in the vacuum housing, 상기 진공발생장치에 의한 진공에 의해서 상기 아세토니트릴과 증류수가 감압여과되도록 된 것을 특징으로 하는 식품내 잔류농약 추출장치.Residual agrochemical extractor in food, characterized in that the acetonitrile and distilled water is filtered under reduced pressure by a vacuum by the vacuum generator. 제 1 항에 있어서, 상기 각 깔대기 상부에 위치되며 상하단부가 개구된 중공컵과, 상기 깔대기와 중공컵을 연결시키는 연결튜브와, 상기 중공컵과 상기 여과지 사이에 마련되어 밀폐시키는 오링과, 상기 깔대기 상단에 마련되어 상기 여과지를 지지시키는 유리섬유를 구비하여 된 것을 특징으로 하는 식품내 잔류농약 추출장치.According to claim 1, wherein the upper and lower ends of the hollow cup located in the upper and lower ends of the funnel, the connecting tube connecting the funnel and the hollow cup, the O-ring provided between the hollow cup and the filter paper and sealed, the top of the funnel Residual pesticide extraction device in the food, characterized in that provided with a glass fiber to support the filter paper. 제 1 항 또는 제 2 항에 있어서, 상기 각 깔대기에 대응하는 턴테이블에는 상기 발생된 진공을 개폐하며 상기 연결관과 연결되는 복수의 조절밸브가 마련되고,According to claim 1 or 2, The turntable corresponding to each funnel is provided with a plurality of control valves for opening and closing the generated vacuum and connected to the connecting pipe, 상기 각 조절밸브에 연결되는 지지관과, 상기 각 지지관의 상단에 지지되며 상기 깔대기가 지지되는 용기수용관과, 상기 각 용기수용관에 수용되어 상기 여과지로부터 용해되는 잔류농약이 수용되는 용기와, 상기 용기수용관과 깔대기 사이를 밀폐하는 밀폐링을 구비하여 된 것을 특징으로 하는 식품내 잔류농약 추출장치.A support tube connected to each of the control valves, a container accommodation tube supported on the top of each of the support tubes and supported by the funnel, a container containing residual pesticide contained in each container accommodation tube and dissolved from the filter paper; , Residual pesticide extracting device in the food, characterized in that provided with a sealing ring for sealing between the container receiving tube and the funnel. 제 1 항 또는 제 2 항에 있어서, 상기 각 제1,2공급호스는 각각 아세트니트릴 저장조와 증류수 저장조에 연결되고,The method of claim 1 or 2, wherein each of the first and second supply hoses are respectively connected to an acetonitrile reservoir and a distilled water reservoir, 상기 각 저장조로부터 아세트니트릴과 증류수가 각각 정량공급모터에 의해서 정량적으로 공급되도록 된 것을 특징으로 하는 식품내 잔류농약 추출장치.Acetic nitrile and distilled water from each of the reservoirs, characterized in that the residual pesticide extracting device in the food, characterized in that the quantitative supply motor.
KR20-2003-0004967U 2003-02-20 2003-02-20 remaining agricultural chemical extraction apparatus in food KR200313049Y1 (en)

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Publication number Priority date Publication date Assignee Title
CN110170180A (en) * 2019-04-18 2019-08-27 广东省测试分析研究所(中国广州分析测试中心) A kind of extracting at constant temperature/extraction Suction filtration device of solid waste/heavy metal in soil Leaching
CN114459792A (en) * 2022-01-20 2022-05-10 合肥高尔生命健康科学研究院有限公司 System for analyzing components of residual pesticide in crops
CN116500214A (en) * 2023-06-06 2023-07-28 吕玉霞 Pesticide residue detection pretreatment system and method
CN116625734A (en) * 2023-07-14 2023-08-22 沈阳海关技术中心 Portable medicine residue detection equipment

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110170180A (en) * 2019-04-18 2019-08-27 广东省测试分析研究所(中国广州分析测试中心) A kind of extracting at constant temperature/extraction Suction filtration device of solid waste/heavy metal in soil Leaching
CN110170180B (en) * 2019-04-18 2021-09-10 广东省测试分析研究所(中国广州分析测试中心) Constant-temperature leaching/extraction suction filtration device for leaching toxicity of heavy metals in solid waste/soil
CN114459792A (en) * 2022-01-20 2022-05-10 合肥高尔生命健康科学研究院有限公司 System for analyzing components of residual pesticide in crops
CN114459792B (en) * 2022-01-20 2023-09-29 合肥高尔生命健康科学研究院有限公司 Residual pesticide composition analysis system in crops
CN116500214A (en) * 2023-06-06 2023-07-28 吕玉霞 Pesticide residue detection pretreatment system and method
CN116500214B (en) * 2023-06-06 2024-02-06 广东省标检产品检测认证有限公司 Pesticide residue detection pretreatment system and method
CN116625734A (en) * 2023-07-14 2023-08-22 沈阳海关技术中心 Portable medicine residue detection equipment
CN116625734B (en) * 2023-07-14 2023-10-03 沈阳海关技术中心 Portable medicine residue detection equipment

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