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A method for the simultaneous determination of acetaminophen and acetaminophen in food of animal origin

A technology of salicylic oxime and salicylic oxime, which is applied in the field of simultaneous determination of salicylic acid and salicylic oxime in animal-derived food, can solve the problems of high false positive rate and inapplicability of qualitative results, and achieves wide applicability, The effect of reducing interference and high sensitivity

Active Publication Date: 2019-11-22
海南特谱农业科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patented method is suitable for fruits and vegetables, but the matrix-dispersed solid-phase extraction method is not suitable for animal-derived foods with complex matrices. In addition, the false positive rate of qualitative results obtained by the SIM method is higher than that of the MRM method.

Method used

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  • A method for the simultaneous determination of acetaminophen and acetaminophen in food of animal origin
  • A method for the simultaneous determination of acetaminophen and acetaminophen in food of animal origin
  • A method for the simultaneous determination of acetaminophen and acetaminophen in food of animal origin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Example 1 Determination of Residual Amounts of Acetamide and Acetamide Oxime in Pork

[0064] (1) Sample pretreatment

[0065] ①Sample preparation: Take about 1 kg of the pork sample to be tested, cut it into small pieces, mash and mix the sample thoroughly with a masher, make a homogenate, put it into a clean container, seal it, and mark it. Store the samples at -18°C.

[0066] ②Extraction: Thaw the sample fully, weigh 5g of pork sample (accurate to 0.01g) into a 50mL centrifuge tube, add 20mL of acetonitrile, 5g of anhydrous sodium sulfate, homogenize at 15000rpm for 2min at high speed, then wash the knife head with 10mL of acetonitrile for 1min, Obtain the homogenized mixture and washing liquid; centrifuge the homogenized mixture at 4 000 rpm for 10 min, collect the supernatant to a 100 mL distillation bottle, add the washing liquid for washing the knife head to the residue, vortex and mix for extraction for 2 min, and centrifuge at 4 000 rpm for 10 min , collect t...

Embodiment 2

[0107] Example 2 Determination of Residual Amounts of Acetamide and Acetamide Oxime in Chicken

[0108] (1) Take the chicken sample to be tested, the pretreatment method of the chicken sample, the preparation method of the standard solution and the blank solution and the determination method are consistent with Example 1. The MRM chromatogram of chicken matrix blank solution is shown in Figures 13 to 14 . The obtained standard working curve is shown in Table 9. image 3 , Figure 4 Shown:

[0109] Table 9 Matrix-matched calibration curves of oxamyl and oxamyl oxime in chicken

[0110] pesticide Retention time / min Matrix-matched calibration curve correlation coefficient kill line 1.53 y=68255x+253428 0.9954 Kill line oxime 1.35 y=71492x+71154 0.9995

[0111] (4) Standard recovery and repeatability

[0112] Add 0.001mg / kg, 0.005mg / kg and 0.02mg / kg standard solutions of 0.001mg / kg, 0.005mg / kg and 0.02mg / kg to the chicken that does not ...

Embodiment 3

[0119] Example 3 Determination of Residual Amounts of Acetamide and Acetamide Oxime in Pig Liver

[0120] (1) The pretreatment and determination methods of pig liver samples are consistent with those in Example 1. The MRM chromatogram of pig liver matrix blank solution is shown in Figures 17-18 , the matrix-matched standard working curves of the obtained sialocarb and syroxyl oxime in pig liver are shown in Table 11, Figure 5 , Image 6 Shown:

[0121] Table 11 Matrix-matched calibration curves of Xanthicarb and Xanthicarb oxime in pig liver

[0122]

[0123]

[0124] (2) Standard recovery and repeatability

[0125] Add 0.001 mg / kg, 0.005 mg / kg and 0.02 mg / kg standard solutions of 0.001 mg / kg, 0.005 mg / kg, and 0.02 mg / kg of the pig liver sample that does not contain saxamyl and saxamyl oxime, and let it stand at room temperature After 30 minutes, carry out pretreatment according to step (1). Among them, pig liver is added with 0.005mg / kg Shaxianwei MRM chromatogr...

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Abstract

The invention discloses a method for simultaneously detecting oxamyl and oxamyl oxime in animal-derived foods. The method comprises the following steps: extracting an animal-derived sample by adopting acetonitrile, and purifying the extract on columella by solid-phase extraction; removing granulated impurities by utilizing low-temperature high-speed centrifuging; efficiently purifying the animal-derived food with complicated substrate to reduce impurity interference and prepare a test sample solution; preparing a substrate match standard solution with series concentration; and simultaneously detecting oxamyl and oxamyl oxime in the sample by utilizing a multi-reaction monitoring (MRM) mode of a liquid chromatography-tandem mass spectrometry. The method has the advantages of low quantification limit, high sensitivity and the like, and has recovery rate and repeatability in accordance with requirement, thus being an effective method for simultaneously detecting residues of oxamyl and oxamyl oxime in animal-derived foods.

Description

technical field [0001] The invention relates to the technical field of food residues, in particular to a method for simultaneously measuring cloxamethasone and oxazacarb oxime in animal source foods. Background technique [0002] Shaxianwei (CAS﹟: 23135-22-0), also known as Oxamyl, English name Oxamyl, chemical name N,N-dimethyl-α-methylcarbamoyloxyimino-α-methylsulfide Acetamide is a carbamate pesticide, which is mainly used as a broad-spectrum insecticide, and has both acaricidal and nematicidal activities. The registered crops of Chisimcarb include citrus, melon, tomato, sweet pepper, cucumber, carrot, potato, peanut and cotton. Shaxianwei is a highly toxic pesticide and has neurotoxicity to the human body. Champa and its metabolites may remain in agricultural products, food or the environment, and have potential health risks to humans. GB2763-2014 stipulates that the maximum residue limit (MRL) of Shaxiancarb in peanut kernels and other foods is 0.05-2mg / kg. Both Chi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/7266
Inventor 阳辛凤罗金辉徐志
Owner 海南特谱农业科技有限公司