ICP-MS (inductively coupled plasma mass spectrometry) Rapid detection method to measure lead and total arsenic in soybean sauce at same time

An ICP-MS and detection method technology, which is applied to the rapid detection of total arsenic by ICP-MS and the simultaneous determination of lead in soy sauce. Emission into the atmosphere, less environmental pollution, and less reagent dosage

Inactive Publication Date: 2018-03-13
INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

These two standard methods and the microwave digestion pretreatment method stipulated in the GB 5009.268-2016 "The First Method for the Determination of Multi-Elements in Food by Inductively Coupled Plasma Mass Spectrometry" implemented on June 23, 2017 require a large one-time investment; Other methods also have the defects of troublesome sample pretreatment, many steps, long time-consuming, many reagents used, heavy pollution, high energy consumption, slow detection speed, and high cost
Especially during the sample pretreatment process, reagents such as strong acids (perchloric acid, nitric acid, etc.) are directly heated and discharged into the atmosphere, resulting in serious environmental pollution. For many laboratories located in old urban areas, this will seriously affect their survival and development

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  • ICP-MS (inductively coupled plasma mass spectrometry) Rapid detection method to measure lead and total arsenic in soybean sauce at same time

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Experimental program
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Effect test

Embodiment 1

[0049] The ICP-MS quick detection method that the present embodiment provides for the simultaneous determination of lead and total arsenic in soy sauce comprises the following steps:

[0050] (1) Sample digestion

[0051] Accurately pipette 0.5mL of soy sauce sample, put it into a 50mL glass centrifuge tube with a ground stopper, add 5mL of nitric acid, quickly add 1mL of hydrogen peroxide, shake gently, mix well, ultrasonically digest for 5-10min, and then in the ground Put the digestion aid A into the glass centrifuge tube, continue ultrasonic digestion for 15-20min, after the ultrasonic is completed, filter;

[0052] Put the filtered filtrate into another 50mL glass centrifuge tube with ground plug, put digestion aid B in the glass centrifuge tube with ground plug, then add 3mL nitric acid and 1mL hydrogen peroxide, shake gently, and mix well , ultrasonic digestion for 5-15min, after the ultrasonication is completed, filter, then add secondary deionized water or distilled ...

Embodiment 2

[0067] Embodiment 2 calibration curve, linear equation and correlation coefficient

[0068] Under optimized spectral mass spectrometry conditions, a series of mixed standard solutions of 0, 1, 2, 5, 10, 20, 40, and 100 μg / L were pumped into the inductively coupled plasma mass spectrometer to determine the analyte and content. The signal response value of the standard element, the concentration of the element to be measured is the abscissa, the ratio of the signal response value of the element to be measured to the selected internal standard element is the ordinate, and the total arsenic-total arsenic and the internal standard element are plotted 72 Standard curve of Ge signal response ratio and Pb-Pb vs internal standard elements 209 For the standard curve of Bi signal response ratio, see figure 1 with figure 2 , its linear curve equation and correlation coefficient are shown in Table 4 and Table 5.

[0069] The results show that the linearity of total arsenic is good in t...

Embodiment 3

[0074] Embodiment 3 The inventive method detection limit and quantitative limit

[0075] The detection limit and quantification limit of the present invention are obtained by using cooking soy sauce and table soy sauce without lead and arsenic as blank samples, and after pretreatment, are measured continuously for 11 times. The detection limit of total arsenic in soy sauce in this scheme is: 0.015mg / L, the quantification limit is: 0.050mg / L, see the following table 6 for details; the detection limit of lead is: 0.015mg / L, the quantification limit is: 0.050mg / L , see Table 7 below for details.

[0076] Table 6 Detection limit and quantification limit of total arsenic

[0077]

[0078]

[0079] Table 7 lead detection limit and quantification limit

[0080]

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Abstract

The invention discloses an ICP-MS (inductively coupled plasma mass spectrometry) rapid detection method to measure lead and total arsenic in soybean sauce at same time, comprising the steps of (1) digesting a sample; (2) detecting with an ICP-MS instrument. The method of the invention has the advantages that chemical reaction conditions are improved, digestion of the sample is accelerated, detection time is shortened, and detection efficiency is improved; the method provides closed and low temperature conditions, rarely causes volatilization loss and mutual pollution interference, is simple, reliable and efficient to perform and has good digestion effect, high detection precision and high accuracy; residual liquid from sample pretreatment is free of heating or emptying, the residual liquidis recycled directly, and low environmental pollution is caused; many samples can be pretreated at a time; reagent consumption is low, equipment power consumption is low, and detection cost is low.

Description

technical field [0001] The invention relates to an ICP-MS rapid detection method for simultaneously determining lead and total arsenic in soy sauce. Background technique [0002] With the rapid development of the food industry and the improvement of people's living standards, unprecedented prosperity and prosperity have occurred in the production and market of condiments. According to reports, in 2012, the output of soy sauce in my country has reached 7 million tons, and the per capita consumption is 5.2 kg, but there is still a big gap from the level of 7.8 kg per capita in Japan. With the upgrading of product structure, the industry growth rate is expected to reach 10-15% in the future . [0003] Lead and arsenic belong to the 10 chemicals of major public health concern listed by the World Health Organization. Among them, the impact of lead on the body is systemic and multi-system, and the main target organs are the nervous system and hematopoietic system. Excessive inta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/38G01N1/44G01N27/64
Inventor 王境堂刘靖靖李宗芮张文皓张帅
Owner INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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