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Method for simultaneously measuring chlorite, chlorate, perchlorate and bromate in ozonization normal saline through IC-MS method

A technology of physiological saline and chlorite, applied in the field of ion chromatography detection, can solve problems such as complicated operation steps, and achieve the effect of simple and quick sample pretreatment method

Inactive Publication Date: 2019-05-21
INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the detection techniques of chlorite, chlorate, perchlorate and bromate are mainly gas chromatography, ion chromatography and other detection techniques, and the operation steps are relatively cumbersome
At present, my country has not yet established an industry standard system for chlorite, chlorate, perchlorate, and bromate in ozonated saline, so a simultaneous determination of chlorite, chloride in ozonated saline has been established. Chlorate, perchlorate, bromate method is of great significance for the protection of human health

Method used

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  • Method for simultaneously measuring chlorite, chlorate, perchlorate and bromate in ozonization normal saline through IC-MS method
  • Method for simultaneously measuring chlorite, chlorate, perchlorate and bromate in ozonization normal saline through IC-MS method
  • Method for simultaneously measuring chlorite, chlorate, perchlorate and bromate in ozonization normal saline through IC-MS method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] This IC-MS method measures the method for chlorite, chlorate, perchlorate, bromate in ozonated normal saline simultaneously, it is characterized in that, comprises the following steps:

[0022] (1) Sample pretreatment; (2) Injection analysis; (3) Qualitative and quantitative analysis.

[0023] The steps of sample pretreatment are as follows: use a syringe to take out ozonated saline and place it in a brown bottle, pipette 100 μl of ozonated saline into the sample vial, then add 900 μl of deionized water, and vortex for 2 minutes directly after analysis.

[0024] The steps of sample injection analysis are as follows:

[0025] (1) IC5000+ (Thermo): mobile phase: KOH; chromatographic column: Dionex#Ion Pac#AS16 type anion analysis column (250mm x2mm, Thermo) equipped with Dionex#Ion Pac#AS16 type anion guard column (50mmx2mm, Thermo); The mobile phase gradient changes as follows: 0-9min 3mmol, 9-11min 25mmol, 11-19min 45mmol, 19-25min 25mmol;

[0026] (2) 4000 Q trap MS...

Embodiment 2

[0028] The linear range, linear equation, correlation coefficient, detection limit, quantitative limit of embodiment 2 method

[0029] In this example, the method provided in Example 1 was used to measure chlorate and perchlorate for certain ozonated saline, and the recovery rate of the method was measured.

[0030] The contents of chlorate and perchlorate in the samples are shown in Table 1 and Table 2.

[0031]

[0032]

[0033]

[0034] For the recovery rate experiment of chlorate, three levels of tests were carried out according to the addition of 100 / 200 / 500ng / mL. Each test was carried out three times. The results are shown in Table 3-5.

[0035]

[0036]

[0037]

[0038]

[0039] For the recovery rate experiment of perchlorate, three levels of tests were carried out according to the addition amount of 0.5 / 1 / 2ng / mL, and each test was carried out three times. The results are shown in Table 6-8

[0040]

[0041]

[0042]

[0043] See Table 9...

Embodiment 3

[0045] Embodiment 3 actual sample detection

[0046] The physiological saline containing 40 μg / ml ozone was taken and tested according to the method of Example 1. It was found through measurement that different types of salts had different response modes on the mass spectrometer. Table 1 shows the IC-MS response modes of different salts in ozonated saline.

[0047] Table 1 Distribution of IC-MS response modes of different salts in ozonated saline

[0048]

[0049]

[0050] figure 1 It is the XIC diagram of ozonated saline No. 5 sample after adding 50ppb standard. Figure 2-5 They are the detection mass spectra of ozonated saline No. 5 sample spiked with 50ppb chlorite, chlorate, perchlorate and bromate.

[0051] After detection and analysis, it was found that the ozonated saline samples mainly contained chlorate and perchlorate, and the content varied with different samples. The content of chlorate and perchlorate can be determined according to the area of ​​the peak...

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Abstract

The invention discloses a method for simultaneously measuring chlorite, chlorate, perchlorate and bromate in ozonization normal saline through an IC-MS method. The method comprises: (1) sample pretreatment; (2) sample introduction analysis; and (3) qualitative and quantitative analysis. The method has advantages that a sample pretreatment method is simple and rapid; the chlorite, the chlorate, theperchlorate and the bromate in the ozonization normal saline are simultaneously measured during one sample introduction; and the qualitative and quantitative analysis of four salts in the normal saline can be realized.

Description

technical field [0001] The invention relates to an IC-MS method for simultaneously measuring chlorite, chlorate, perchlorate and bromate in ozonated physiological saline, belonging to the field of ion chromatography detection. Background technique [0002] In recent years, the clinical role of ozone therapy has been paid more and more attention. Dissolving ozone in normal saline to form ozonated normal saline can overcome the inherent defects of ozone. Ozonated normal saline can undergo various chemical reactions with body tissue internal fluid, and can produce a variety of highly oxidizing substances, including hydroxyl structures and Monoatomic oxygen, ozonated saline also contains a small amount of ozone molecules, so the oxidation and direct damage of ozonated saline are stronger than that of ozone gas, and it has more advantages in anti-inflammatory and bactericidal aspects. It is used in clinical It is also safer than ozone in treatment. Excessive levels of chlorite,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 崔鹤尹秀贞蔡峰张涛
Owner INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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