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Method for measuring lead content in soybean sauce through microwave digestion-graphite furnace atomic absorption

A graphite furnace atomic and microwave digestion technology is applied in the field of food analysis, which can solve the problems of detection limit and experimental cost limitation, background value affecting lead determination, and obtaining accurate and stable results, etc. Interfering, enhancing stability effects

Inactive Publication Date: 2017-03-15
SHANDONG INST FOR FOOD & DRUG CONTROL
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Problems solved by technology

National standard GB5009.12-2010 lead in food is graphite furnace atomic absorption method, lead detection methods also include flame atomic absorption method, atomic fluorescence method, dithizone colorimetric method and ICP-MS and other methods, but these methods are subject to inspection Larger limitations of factors such as limit and experiment cost
[0003] Graphite furnace atomic absorption spectrometry is an accurate and economical method for the determination of lead at present, but the determination of elements by graphite furnace will be interfered by the matrix in the sample, but soy sauce contains high sodium chloride, and the high content of sodium chloride is higher than that of lead. There is a large background value in the determination that affects the determination of lead, and accurate and stable results cannot be obtained

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  • Method for measuring lead content in soybean sauce through microwave digestion-graphite furnace atomic absorption

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Embodiment 1

[0034] 1) Microwave treatment of samples: Weigh 2.00g of two soy sauces (sample 1 and sample 2) with different lead contents respectively, add 8ml of nitric acid and 2mL of hydrogen peroxide into a polytetrafluoroethylene digestion tank, and digest them in a microwave digestion apparatus , the microwave digestion program is 120°C for 10 minutes, 160°C for 20 minutes, 190°C for 20 minutes, and the power is 1200W; after the digestion is completed, rinse the lid and inner wall of the digestion tank with ultrapure water, and then wash the acid on the acid-removing electric heating plate at 160°C for 90 minutes.

[0035] 2) Preparation of standard solution: Take 10ml of lead standard product with a concentration of 1000mg / L in a 100ml volumetric flask, use 2% nitric acid aqueous solution to make up the volume, and then use 2% nitric acid aqueous solution to dilute to 20µg / ml lead standard solution, and gradually dilute to obtain a 20ng / mL standard solution dilution, for subsequent u...

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Abstract

The invention relates to a method for measuring lead content in soybean sauce through microwave digestion-graphite furnace atomic absorption. The method comprises the following steps: weighing a defined amount of sample and putting into a polytetrafluoroethylene digestion tank; adding nitric acid and hydrogen peroxide; performing digestion pretreatment in a microwave digestion instrument; respectively taking the digested sample, palladium nitrate in mass percent of 10% and ammonium dihydrogen phosphate in mass percent of 10% and jointly injecting into a pyrolytic coating graphite tube for measuring. According to the method provided by the invention, the influence of soybean sauce substrate on lead measurement can be effectively reduced, the stability and precision of the method can be increased and the test process is simple, quick, sensitive and accurate. The method is suitable for the measurement for the lead content in soybean sauce and daily food, such as, pickle, salt, vegetable and milk powder.

Description

technical field [0001] The invention belongs to the technical field of food analysis and relates to a microwave digestion-graphite furnace atomic absorption method for determining the lead content in soy sauce. Background technique [0002] Lead is an accumulative element, an important indicator in food hygiene standards, and a metal element that is harmful to the human body, especially to the growth and intellectual development of children. [ . Soy sauce is a seasoning product, which is widely used in daily life, so it is of great significance to detect lead in soy sauce. National standard GB5009.12-2010 lead in food is graphite furnace atomic absorption method, lead detection methods also include flame atomic absorption method, atomic fluorescence method, dithizone colorimetric method and ICP-MS and other methods, but these methods are subject to inspection Larger limitations of factors such as limit and experiment cost. [0003] Graphite furnace atomic absorption spect...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N1/44
CPCG01N1/44G01N21/3103
Inventor 赵发刘艳明董瑞于文江张喜琦祝建华徐大玮
Owner SHANDONG INST FOR FOOD & DRUG CONTROL
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