Pretreatment method for detecting chloramphenicol in milk or mild products and method for detecting chloramphenicol in milk or mild products
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A technology for chloramphenicol and dairy products, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as low detection recovery rate and inability to effectively eliminate impurity interference.
Inactive Publication Date: 2013-01-30
INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD
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However, with the usual pretreatment method, the detection recovery rate is not high, and the impurity interference cannot be effectively eliminated.
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Embodiment 1
[0027] 1) Preparation of standard solution:
[0028] Accurately weigh 10 mg of each chloramphenicol standard substance, dilute it in a 100 mL brown volumetric flask with methanol, and mix well to obtain a standard stock solution with a chloramphenicol concentration of 0.1 mg / mL, and store it in a -18°C freezer in the dark. Good for at least 4 weeks. When in use, dilute to 5.0ng / mL, 1.0ng / mL, 0.5ng / mL, 0.3ng / mL, 0.1ng / mL standard solution. It is also possible to prepare multiple standard solutions at concentrations different from the above.
[0029] 2) Preparation of mobile phase:
[0030] Mobile Phase A: Methanol
[0031] Mobile phase B: 0.1% formic acid in water
[0032] 3) Preprocessing method:
[0033] Weigh 5.00g of milk sample, add 15mL of ethyl acetate, process it with a vortex device for 1min, put it into an ultrasonic machine for ultrasonic treatment for 20min, and centrifuge it at 14000r / min for 10min, take 10mL of the supernatant, and place it under nitrogen In...
Embodiment 2
[0065] The chloramphenicol spiked samples with a concentration of 1.0 μg / Kg were dissolved in ultrapure water, 5% methanol solution, 10% methanol solution, 15% methanol solution, and 20% methanol solution to obtain 5 different the first solution.
[0066] Take 5 solid-phase extraction cartridges, use 5.0mL methanol to pass through each solid-phase extraction cartridge at a flow rate of 1.0-2.0mL / min, and then use 5.0mL ultrapure water to pass through each solid-phase extraction cartridge at a flow rate of 1.0-2.0mL / min. Phase extraction cartridges, the above five different first solutions were purified and enriched through five solid phase extraction cartridges at a flow rate of 1.0-2.0mL / min, and then 5.0mL of ultrapure water was used at 1.0 The flow rate of ~2.0mL / min passes through each solid-phase extraction column, and the solid-phase extraction column is drained with a vacuum pump; 3mL of methanol and 3mL of ethyl acetate are added to the solid-phase extraction column en...
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Abstract
The invention relates to a pretreatment method for detecting chloramphenicol in milk or mild products, comprising the following steps: adding a sample extracting agent to a sample to obtain a sample extracting solution, letting the sample extracting solution successively be subject to vortex treatment, ultrasonic treatment and centrifugation to obtain a supernatant, drying the supernatant to obtain substances, and then dissolving the substances with a methanol solution having the concentration of 10% to obtain a first dissolved solution; successively using methanol and untrapure water to flow through a solid-phase extraction cartridge, then purifying and gathering the first dissolved solution through the solid-phase extraction cartridge, and then using untrapure water to flow through the solid-phase extraction cartridge, and then draining the solid-phase extraction cartridge; then respectively adding equal parts of methanol and ethyl acetate in the drained solid-phase extraction cartridge for eluting, collecting the eluent and drying the eluent, dissolving with a methanol solution having the concentration of 50% to obtain a second dissolved solution, carrying out vortex treatment on the second dissolved solution, and then filtering with a microporous filtering membrane. According to the invention, the recovery rate of the detection can be raised, and the interference of impurity can be effectively eliminated.
Description
technical field [0001] The invention relates to a method for detecting antibiotic content in milk and dairy products, in particular to a pretreatment method for detecting chloramphenicol in milk or dairy products, and also relates to a detection of residual chloramphenicol in milk and dairy products method. Background technique [0002] Chloramphenicol (CAP) is a chloramphenicol antibiotic (Chloramphenicols, CAPs), which is commonly used in veterinary clinics. Its main side effect is to inhibit hematopoietic function and cause irreversible aplastic anemia. [0003] At present, in order to detect chloramphenicol in milk or dairy products, the usual pretreatment method is to use solid phase extraction to extract and purify chloramphenicol in the sample. However, with the usual pretreatment method, the detection recovery rate is not high, and the impurity interference cannot be effectively eliminated. Contents of the invention [0004] The purpose of the present invention i...
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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/14
Inventor 崔涛张雪峰常建军李梅刘卫星
Owner INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD
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