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Joint extraction and detection method of inorganic iodine and organic iodine in kelp

A technology of combined extraction and detection methods, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as the inability to detect multiple iodine contents at the same time, and achieve reduction of human health and environmental hazards, high extraction efficiency, and high sensitivity Effect

Inactive Publication Date: 2019-05-03
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Disclosed " a kind of iodine content detection method in feedstuff " on Chinese patent document, its notification number is CN104458965A, this invention adopts iodate radical to have strong oxidation property under acidic condition, adopts under dilute sulfuric acid condition, adds excessive sodium metabisulfite, All the iodine in the sample is reduced to iodide ion, and then the iodide ion in the solution is determined by ion-pair chromatography, but this invention cannot detect multiple iodine contents at the same time

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  • Joint extraction and detection method of inorganic iodine and organic iodine in kelp
  • Joint extraction and detection method of inorganic iodine and organic iodine in kelp
  • Joint extraction and detection method of inorganic iodine and organic iodine in kelp

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1. The combined extraction and detection of inorganic and organic iodine in kelp from Shandong:

[0034] Accurately weigh 1.0 g of a sample of kelp granules from Shandong province and place them in a 50 mL conical flask, add 10 mL of 200 mM ethyl pyridine bromide ([EPy]Br) ionic liquid, adjust the pH to 6.5, and set it at 40°C Extract for 30 minutes in an ultrasonic instrument under temperature conditions, centrifuge the mixture (4000rpm, 10 minutes), carefully collect the supernatant for ultra-high performance liquid chromatography (UHPLC) analysis:

[0035] The chromatographic analysis of MIT, DIT and KI was performed on Agilent 1290 Ultra Performance Liquid Chromatography (Santa Clara, USA). The chromatographic column is an Agilent Zorbax SB C18 column (5μm, 4.6×150mm), and the column temperature is kept at 22°C. The mobile phase consisted of 10mM KH2PO4 (A) and acetonitrile (B), and the flow rate was set to 0.5mL / min.

[0036] The gradient elution procedure is as...

Embodiment 2

[0041] Example 2. Combined extraction and detection of inorganic iodine and organic iodine in kelp produced in Fujian

[0042] The difference between embodiment 2 and embodiment 1 is that the detection object is kelp whose origin is Fujian, and the other process conditions are completely the same.

[0043] figure 1 UHPLC chromatograms of three 50μg / mL iodine standards, image 3 The UHPLC chromatogram of the kelp extract produced in Fujian in this example, combined figure 1 with image 3 It can be seen that MIT, DIT and KI were successfully extracted from the obtained extract.

[0044] The peak area of ​​each analyte in the extract of this example is shown in Table 2:

[0045] Table 2.

[0046] Analyte

Embodiment 3

[0047] Example 3. Combined extraction and detection of inorganic iodine and organic iodine from kelp produced in Zhejiang Province. The difference between Example 2 and Example 1 is that the detection object is kelp produced in Zhejiang Province, and the rest of the process conditions are exactly the same.

[0048] figure 1 UHPLC chromatograms of three 50μg / mL iodine standards, Figure 4 The UHPLC chromatogram of the kelp extract produced in Zhejiang Province of this example, combined figure 1 with Figure 4 It can be seen that MIT, DIT and KI were successfully extracted from the obtained extract.

[0049] The peak area of ​​each analyte in the extract of this example is shown in Table 3:

[0050] table 3.

[0051] Analyte

KI

MIT

DIT

Peak area

6389.3

9.0

6.3

[0052] Intraday precision

[0053] Accurately weigh 1.0g of the ground particle sample and place it in a 50mL Erlenmeyer flask, then add 10mL of 200mM [EPy]Br solution into the Erlenmeyer flask, adjust the pH value of the...

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Abstract

The invention relates to the technical field of natural medicine extraction detection and provides a joint extraction and detection method of inorganic iodine and organic iodine in kelp, thereby solving a problem that several kinds of iodine can not be measured simultaneously by the traditional iodine extraction detection process. The inorganic iodine is potassium iodide and the organic iodine is3-iodo-L-tyrosine and 3,5-diiodo-L-tyrosine. Moreover, the method comprises the following steps: weighing 1.0g of mashed kelp particle samples precisely; adding 10mL of ionic liquid and adjusting thepH value to be 5.0 to 7.0; carrying out extraction for 15 to 75min in ultrasound equipment at a temperature of 40 DEG C; carrying out centrifugation and collecting supernate; and carrying out ultra-high-performance liquid chromatogram analysis and detection. According to the invention, the ILs is used as the LSE extraction solvent; the biologically active iodine is extracted from a complex samplematrix rapidly and efficiently by using a simple and economic device during the single process; and I<->, MIT and DIT inorganic and organic iodine in actual samples can be extracted and detected simultaneously. The extraction time is short; the detection limit is low; the green and environment-friendly effects are good; and the satisfying extraction efficiency is obtained.

Description

Technical field [0001] The invention relates to the technical field of extraction and detection of natural medicines, in particular to a combined extraction and detection method of inorganic iodine and organic iodine in kelp. Background technique [0002] Iodine was discovered by French chemist Courtois in 1811 and is a naturally occurring non-metallic element in group VIIA of the periodic table. As an essential trace element, iodine is vital to the healthy development of animals and humans. As a component of thyroid hormones, iodine deficiency can cause severe delays in neurodevelopment in children, as well as goiter and hypothyroidism in adults. Therefore, the exact concentration of different iodine substances in daily diet and water has considerable scientific significance. In nature, iodine has various inorganic and organic forms, including iodide, iodate and organic iodine (tetraiodothyronine (T4), triiodothyronine (T3), diiodothyronine Acid (T2), 3-iodo-L-tyrosine (MIT) ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 曹君胡雨涵王秋燕杨娟彭黎卿董新杜丽晶
Owner HANGZHOU NORMAL UNIVERSITY
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