Method for determining residual quantity of chloramphenicol in bee wax by n-hexane pre-treatment-high performance liquid chromatography-tandem mass spectrometry

A technology of high performance liquid chromatography and tandem mass spectrometry, applied in the field of determination of chloramphenicol residues in beeswax, can solve the problems of complex beeswax matrix and inability to use detection

Inactive Publication Date: 2015-09-02
衢州出入境检验检疫局综合技术服务中心
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Problems solved by technology

Due to the complex matrix of beeswax, it is impossible to detect chloramphenicol in honey, royal jelly and other bee products published at home and abroad.

Method used

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  • Method for determining residual quantity of chloramphenicol in bee wax by n-hexane pre-treatment-high performance liquid chromatography-tandem mass spectrometry
  • Method for determining residual quantity of chloramphenicol in bee wax by n-hexane pre-treatment-high performance liquid chromatography-tandem mass spectrometry
  • Method for determining residual quantity of chloramphenicol in bee wax by n-hexane pre-treatment-high performance liquid chromatography-tandem mass spectrometry

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Experimental program
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Embodiment Construction

[0026] 1 Experimental part

[0027] 1.1 Instruments and reagents

[0028] Ultimate 3000 ultra-high performance liquid chromatography-TSQ Vantage triple quadrupole tandem mass spectrometer (Thermo Scientific, USA); MS 3 digital vortex mixer (IKA, Germany); MD 200 nitrogen blowing instrument (Hangzhou Aosheng Instrument Co., Ltd.)

[0029] Chloramphenicol (CAS56-75-7, purity ≥ 98%) and chloramphenicol-D5 (purity ≥ 98%), Dr. Ehrenstorfer Company. Methanol, n-hexane, and ethyl acetate were all chromatographically pure; OASIS HLB solid-phase extraction cartridge: 500 mg, 6 mL (Waters, USA).

[0030] 1.2 Preparation of standard solution

[0031] Weigh 10 mg of chloramphenicol standard substance (accurate to 0.1 mg) and place it in a 100 mL brown volumetric flask, dissolve it with methanol and dilute to the mark, and mix well to prepare a 100 mg / L standard stock solution. Prepare a 1mg / L single-standard stock solution with methanol, and dilute it with fluidity to form a correspond...

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Abstract

The invention relates to a method for determining the residual quantity of chloramphenicol in bee wax by n-hexane pre-treatment-high performance liquid chromatography-tandem mass spectrometry. The method comprises the following steps: pre-dissolving a test sample by adopting n-hexane to form emulsion, and adding water and extracting; carrying out HLB (Hydrophile Lipophile Balance) solid-phase extraction column purification; separating by using an Accucore XL C18 column; and determining by using electric spraying ion source negative ion multi-reaction monitoring mode tandem mass spectrum. Extraction and purification methods, and instrument determination conditions and the like are optimized. A result shows that chloramphenicol has a relatively good linear relation in a range of 0.3ng/mL-10ng/mL, and the correlation coefficient is more than 0.998. The method qualitative limit (S/N>3) is 0.05 microgram/kilogram and the method quantitative limit (S/N>10) is 0.3 microgram/kilogram; the recycling rate of three adding levels of 0.3 microgram/kilogram, 1.0 microgram/kilogram and 2.0 microgram/kilogram is 80.2%-105.2%; and the relative standard deviation (RSD, n=6) is smaller than 8%. The method is rapid, sensitive and accurate.

Description

technical field [0001] The invention relates to a method for determining the residual amount of chloramphenicol in beeswax. Background technique [0002] Chloramphenicol (CAP) is a high-efficiency broad-spectrum antibiotic that is active against various aerobic and anaerobic microorganisms and is widely used in animal husbandry. However, chloramphenicol has certain toxic effects on humans, such as causing human agranulocytosis, aplastic anemia and allergies and other symptoms. FAO / WAO stipulates that the residues of chloramphenicol in food shall not be detected, and the European Union (EEC) Directive 96 / 23 lists CAP as a banned drug, and stipulates that the MRPL (minimum required performance limits) value of chloramphenicol is 0.3 μg / kg. [0003] my country is a major beekeeping country in the world, as well as a major producer and exporter of bee products. In 2013, the total output of beeswax was about 8,000 tons. Beeswax is a substance secreted by four pairs of wax gland...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 雷美康彭芳徐佳文余琪祝子铜吴晓勤
Owner 衢州出入境检验检疫局综合技术服务中心
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