Method for simultaneously separating and determining various organic tin and inorganic tin in tobacco

A simultaneous separation and organotin technology, applied in the field of chromatographic analysis and detection, can solve the problems of chromatographic peak tailing, passivation, inability to obtain accurate and reliable quantitative results, etc.

Active Publication Date: 2020-10-16
SHANGHAI TOBACCO GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Leng Taohua et al. reported a method for the determination of various organotins in aquatic products by using HPLC-ICP-MS (Leng Taohua, Chen Guiyu, Duan Wenfeng, etc. High performance liquid chromatography-inductively coupled plasma mass spectrometry analysis of the form of organotins in aquatic products [J]. Analytical Chemistry, 2015,43(4):558-563), although this method can simultaneously detect organotin compounds in aquatic products, there are some important inherent defects: (1) This method cannot simultaneously detect more common (2) Triethylamine must be added as a masking agent in the mobile phase of this method, otherwise the chromatographic peak will have serious tailing, which will greatly increase the detection time and may result in reduced quantitative accuracy
Low-pressure ion chromatography uses atmospheric pressure peristaltic pump instead of high-pressure pump. Its maintenance and use costs are low, but the actual separation effect is poor (see accompanying drawing 3 of its manual), and there is a significant gap compared with high-performance liquid chromatography: low-pressure ion chromatography is difficult to separate tobacco. The more common forms of tin such as tricyclohexyltin (TChT) and tin triazolium (ACT) in the compound are more common; when separated by low-pressure ion chromatography, it is difficult to achieve baseline separation of the compounds to be tested, and the peaks are severely deformed, and there are peak passivation, Inherent defects that are difficult to solve such as peak tailing and peak asymmetry (see Figure 3 of its specification), especially for the analysis of trace metal elements, cannot obtain accurate and reliable quantitative results

Method used

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  • Method for simultaneously separating and determining various organic tin and inorganic tin in tobacco
  • Method for simultaneously separating and determining various organic tin and inorganic tin in tobacco
  • Method for simultaneously separating and determining various organic tin and inorganic tin in tobacco

Examples

Experimental program
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Effect test

Embodiment 1

[0100] 1. Sample pretreatment

[0101] Grind the tobacco sample with a heavy metal special grinder and pass it through a 100-mesh sieve. After balancing for 24 hours in a constant temperature and humidity box with a temperature of (22±1)°C and a relative humidity of (60±2)%, accurately weigh 1g ( Accurate to 0.001g) Tobacco samples in 60mL PET vials, add 10mL of extracting solution, vortex and shake at 50°C for 20min, centrifuge at 3500r / min for 10min, take the supernatant, and concentrate to 1mL by nitrogen blowing . Then filter through a 0.22 μm organic syringe filter to obtain the sample solution. During the processing of tobacco samples, a blank control test was performed simultaneously.

[0102] Wherein, the ratio of the mass (g) of the tobacco sample added to the volume (mL) of the extract is 1:10. The extract is solution A and solution B with a volume ratio of 1:1, wherein solution A is a mixed solution of citric acid, water, and ammonia with a mass ratio of 100:70:0...

Embodiment 2

[0126] As shown in 2 of Example 1 above, accurately pipette the organotin mixed standard stock solution and the inorganic tin standard stock solution respectively, add the extract and dilute to constant volume to prepare a series of mixed standard solutions with different concentrations. In the same mixed standard solution, the contained triphenyltin (TPhT), tributyltin (TBT), tricyclohexyltin (TChT), triazotin (ACT), fenbutyltin (FBT), tin element (Sn) The concentrations are all at the same concentration, that is, a series of mixed standard solutions of 0.5μg / L, 2.0μg / L, 5.0μg / L, 20.0μg / L, 50.0μg / L, and 200.0μg / L were prepared respectively . At the same time, the extract was added to prepare a solution with the concentration of 0 μg / L of the six organic tin and inorganic tin components as a solvent blank.

[0127] A series of mixed standard solutions with different concentrations prepared above were analyzed by high-performance liquid chromatography-inductively coupled plasm...

Embodiment 3

[0133] According to the pretreatment and measurement steps in Example 1, select the low, medium and high three standard addition levels of the tobacco sample, and carry out the mensuration of the sample standard addition recovery rate, and the standard addition amounts are respectively 10ng / g, 50ng / g, 200ng / g, The corresponding recoveries are shown in Table 4. The recovery rate was calculated by the difference between the concentration of the known sample and the spiked sample relative to the amount of the spiked sample, and the recovery rate was between 72.6 and 96.4%, and the recovery rate of the six forms of tin components was better.

[0134] Simultaneously, the recoveries of 6 kinds of tin components of morphologies are continuously carried out 6 parallel determinations, and the corresponding relative standard deviation data are shown in Table 4. The relative standard deviations (RSD) of 6 kinds of morphological tin components are all below 8.0%, illustrating the precision...

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Abstract

The invention provides a method for simultaneously separating and determining various organic tin and inorganic tin in tobacco. The method comprises the following steps: adding a tobacco sample into an extracting solution, oscillating, extracting, centrifuging, taking supernatant, concentrating, filtering to obtain a sample solution, determining by adopting a high performance liquid chromatography-inductively coupled plasma mass spectrometry method, and calculating the contents of various organic tin and inorganic tin in the sample solution by adopting a standard curve method. According to themethod for simultaneously separating and determining various organic tin and inorganic tin in tobacco, organic tin and inorganic tin in complex matrixes such as tobacco can be rapidly and reliably detected at the same time, harm to the body of an operator is reduced, and a technical support is provided for comprehensively and objectively evaluating the harm of tin in tobacco.

Description

technical field [0001] The invention belongs to the technical field of chromatographic analysis and detection, and relates to a method for simultaneously separating and measuring various organic tins and inorganic tins in tobacco, in particular to a method using high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP -MS) simultaneously separates and measures the method for multiple organotins and inorganic tins in tobacco. Background technique [0002] Tin is a common heavy metal element widely distributed in nature, and its compounds are also used in various fields of industry and agriculture. Most inorganic tin compounds are low or slightly toxic, while organotin compounds have high neurotoxicity and can be used as insecticides or bacteriostats, and related studies have reported that they can be used to inhibit tobacco mosaic virus. However, there are few studies on the separation and quantification of tin elements in the tobacco ind...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/72G01N30/86B01J20/281
CPCG01N30/48G01N30/02G01N30/06G01N30/34G01N30/36G01N30/7253G01N30/8679G01N2030/042
Inventor 田志章邢立霞张春涛叶鸿宇李登科吴若昕马立超
Owner SHANGHAI TOBACCO GRP CO LTD
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