CN102879494A - High performance liquid chromatography quantitative determination method of boric acid in water-based adhesive - Google Patents
High performance liquid chromatography quantitative determination method of boric acid in water-based adhesive Download PDFInfo
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- CN102879494A CN102879494A CN2012103629764A CN201210362976A CN102879494A CN 102879494 A CN102879494 A CN 102879494A CN 2012103629764 A CN2012103629764 A CN 2012103629764A CN 201210362976 A CN201210362976 A CN 201210362976A CN 102879494 A CN102879494 A CN 102879494A
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Abstract
The invention discloses a high performance liquid chromatography quantitative determination method of boric acid in a water-based adhesive. The method comprises the following steps: (1) weighing a water-based adhesive sample, adding water, dissolving in a triangular flask to obtain a solution, then performing ultrasonic vibration and centrifugation; (2) adding the supernatant liquor of the solution into a triangular flask, adding a developer solution into the triangular flask, well mixing, drying by distillation in a water-bath kettle; adding a solvent, transferring the solution into a volumetric flask, diluting with the solvent to reach the scale, well mixing; (3) analyzing the solution by a high performance liquid chromatograph; (4) performing quantification by an external standard method with the relation that the peak area is proportional to the concentration. The method adds a curcumin-oxalic acid developer into the sample after dilution, ultrasonic vibration and centrifugation, and puts the sample in a constant-temperature water bath in a water-bath kettle. The solid obtained after drying by distillation is dissolved by the solvent and reaches a constant volume in the volumetric flask. The peak area of a boron-curcumin complex is determined by high performance liquid chromatography, and the boric acid content is calculated by comparison with a standard curve. The method is rapid, reliable, simple and practical.
Description
Technical field
The present invention relates to a kind of high performance liquid chromatography method for quantitatively determining of water base adhesive mesoboric acid.
Background technology
Boric acid is white crystalline powder or colourless little scale with pearl shape gloss, and pungency is arranged, and can and produce cockroach, beetle pesticide as chemical reagent, pharmaceutically is being used as hemostasis and antiseptic.After absorbing via food, borax can produce boric acid with the hydrochloric acid in gastric juice effect.Boric acid is not allowed to as food additives, but among the people often have borax or boric acid are mixed the phenomenon of using as the desinsection antiseptic in the grain, also have in one's early years with boric acid as food preservative and leavening agent problem.For the latex mesoboric acid, dual mode is generally taked in the preservation of latex, and a kind of is that high ammonia is preserved, and a kind of is that low ammonia is engaged between the 0.2-0.25% boric acid of content and preserves.
High performance liquid chromatography is a kind of Modern Chromatographic Analysis method that grows up on the basis of classical liquid chromatography late 1960s, different calls once occurs in history, such as high pressure liquid chromatography, high-speed liquid chromatography and high resolution liquid chromatography.With regard to separation principle, high performance liquid chromatography has adopted the mutually fixing and high sensitivity detector of high pressure pump, high efficiency particle, and high performance liquid chromatography has that analysis speed is fast, separation efficiency good, detection sensitivity is high, analysis speed is fast, sample reclaims and makes things convenient for and the operating automation degree advantages of higher.The method obtains a wide range of applications in bioengineering, pharmaceuticals industry, food industry, environmental monitoring and field of petrochemical industry.
At present the mensuration of domestic efficient liquid-phase chromatography method about boric acid has the part report.
Sui met the content that the people such as army have reported Borax in Bingpeng San by RP-HPLC in 2002.Set up the content of Borax in Bingpeng San by RP-HPLC.Borax is at sample size 0.14～0.71 μ gm as a result]
-1Good linear relationship is arranged, r=0.9992 in the scope.It is easy that conclusion is set up content assaying method, accurately, and favorable reproducibility.
The people such as Chen Yan had reported the rp-hplc method of borax in the food in 2007.Set up reversed-phase high-performance liquid chromatography (RP-HPLC) and measure the method for borax in the food, detecting of method is limited to 6.4ng/kg, and RSD is 2.3%, and the recovery is 90.63%～96.88%, and the range of linearity is 0.032-0.32 μ g/L, and related coefficient is 0.9992.
The people such as nineteen ninety-five Hu Qizhi have reported High Performance Liquid Chromatography Study and the application of boron-curcumin complex compound.Studied complex compound that in non-aqueous system boron and protonated curcumin form take absolute methanol as solvent, the C18 chromatographic column with methanol-water (80: 20V/V) do that mobile phase (1.00mL/min) separates and detect. the calibration curve range of linearity of boron is 0.4～3.2 μ g/25mL, the school of boron is surveyed and is limited to the analysis that this method of 0.08ng. is used for compound boron fertilizer, and the result is satisfactory.
The pre-treating method of these methods adopts the protonated method of concentrated sulphuric acid nitration mixture to process that laggard high performance liquid chromatograph measures more, yet.The concentrated sulphuric acid has certain danger to the operator, and is easy to instrument and equipment is caused corrosion,
At present, about the assay method of water base adhesive mesoboric acid, document rarely has report, and this assay method safely, is easily gone and can injury to instrument and equipment.But have the advantages such as the favorable reproducibility manipulation type is strong for measuring water base adhesive mesoboric acid content.
Summary of the invention
The invention discloses a kind of method with Water By High Performance Liquid base glue mesoboric acid.It is characterized in that the method may further comprise the steps:
(1) take by weighing the water base adhesive sample, adding water is dissolved in and obtains solution in the triangular flask, and then sonic oscillation is centrifugal;
(2) get in the supernatant liquor adding triangular flask of mentioned solution, in triangular flask, add chromogenic reagent solution, mix afterwards evaporate to dryness on water-bath; Add solvent and be transferred in the volumetric flask, with solvent dilution to scale, mixing;
(3) solution liquid adopts high performance liquid chromatograph to analyze;
(4) adopt the relation of peak area and concentration direct ratio quantitative with external standard method.
The sample weighting amount of the water base adhesive sample of described step (1) is 0.1-2g; The volume that adds entry is 10-1000mL, sonic oscillation time 10-30min; Centrifuge speed 4000-12000 turns; Centrifugation time is 5-30min.
The solution supernatant liquor is got 0.1-2mL in the described step (2); Chromogenic reagent solution is the curcumin oxalic acid solution, and the consumption of developer is 2-8mL.
Described step (2) water-bath temperature is the 30-60 degree, and the volumetric flask volume is 20-100mL.
In the described step (2) solvent be in methyl alcohol, 95% ethanol or the absolute ethyl alcohol any one.
Described step (3) chromatographic column adopting reverse-phase chromatographic column, mobile phase ratio: methyl alcohol: water=10-90: 90-10, chromatographic column column temperature: 20-35 ℃; The high performance liquid chromatography coutroi velocity is at 0.2～1mL/min; The employing UV-detector detects, and detects wavelength: 500-600nm.
Compared with prior art, beneficial effect of the present invention is: the determination step of the method is through dilution, ultrasonic, adds curcumin-oxalic acid developer water bath with thermostatic control on water-bath in the sample after centrifugal.The solid that obtains behind the evaporate to dryness uses the dissolution with solvents constant volume in volumetric flask.Adopt the peak area of high effective liquid chromatography for measuring boron-curcumin complex compound, thereby the reference standard curve calculates the content of boric acid.The method fast and reliable, simple.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Described embodiment helps to understand the present invention, and should not be considered as concrete restriction of the present invention.
(1) determination
Accurately take by weighing 1g water base adhesive sample, add 50mL water and be dissolved in the 100mL triangular flask sonic oscillation 10min, centrifugal 10min.Get the 3mL supernatant liquor and add in the triangular flask,
(2) solution preparation
After five times of above-mentioned clear liquid dilutions, in triangular flask, add chromogenic reagent solution, after mixing, evaporate to dryness on 55 degree water-baths adds ethanol and is transferred in the 25mL volumetric flask, is diluted to scale with ethanol, mixing.
(2) solution liquid adopts high performance liquid chromatograph to analyze.
According to the determined method of the present invention, with mentioned solution, injection liquid chromatography behind 0.45 μ m filtering with microporous membrane selects chromatographic condition to measure, and can obtain the content of water base adhesive mesoboric acid.
Embodiment 1
According to method preparation boric acid standard solution described above, with standard solution obtained above injection liquid chromatography behind 0.45 μ m filtering with microporous membrane, according to the determined method of the present invention, under chromatographic condition as described below, measure.
It is good that the result demonstrates the peak, and the chromatographic peak of boric acid separates fully with other component chromatographic peaks.
Wherein, chromatographic column: Extend-C18; Mobile phase: methyl alcohol: water (90: 10 volume ratios); Chromatographic column temperature: 25 ℃; Sample size: 5 μ L; Flow velocity: 1mL/min; Detecting device: UV-detector; Detect wavelength: 550nm.
Embodiment 2
According to method preparation water base adhesive sample solution described above, with standard solution obtained above injection liquid chromatography behind 0.45 μ m filtering with microporous membrane, according to the determined method of the present invention, under chromatographic condition as described below, measure.
It is good that the result demonstrates the peak, and the chromatographic peak of boric acid separates fully with other component chromatographic peaks.
Wherein, chromatographic column: Rx-C18; Mobile phase: methyl alcohol: water (80: 20 volume ratios); Chromatographic column temperature: 35 ℃; Sample size: 10 μ L; Flow velocity: 0.8mL/min; Detecting device: UV-detector; Detect wavelength: 550nm.
Embodiment 3
Take by weighing 0.5g water base adhesive sample, add 50mL water and be dissolved in the 100mL triangular flask, ultrasonic 5min is through the centrifugal 5min of hydro-extractor.Get the 2mL supernatant liquor and add in the triangular flask, with solution obtained above injection liquid chromatography behind 0.45 μ m filtering with microporous membrane, according to the determined method of the present invention, under chromatographic condition as described below, measure.
It is good that the result demonstrates the peak, and the chromatographic peak of boric acid separates fully with other component chromatographic peaks.
Wherein, chromatographic column: Ecl ipse XDB; Mobile phase: methyl alcohol: water (85: 15 volume ratios); Chromatographic column temperature: 30 ℃; Sample size: 20 μ L; Flow velocity: 0.7mL/min; Detecting device: UV-detector; Detect wavelength: 550nm.
Embodiment 4
Take by weighing 1g water base adhesive sample, add 100mL water and be dissolved in the 250mL triangular flask, vibration 15min is through the centrifugal 15min of hydro-extractor.Get the 0.5mL supernatant liquor and add in the triangular flask, with solution obtained above injection liquid chromatography behind 0.45 μ m filtering with microporous membrane, according to the determined method of the present invention, under chromatographic condition as described below, measure.
It is good that the result demonstrates the peak, and the chromatographic peak of boric acid separates fully with other component chromatographic peaks.
Wherein, chromatographic column: Ecl ipse Plus; Mobile phase: methyl alcohol: water (75: 15 volume ratios); Chromatographic column temperature: 30 ℃; Sample size: 10 μ L; Flow velocity: 0.85mL/min; Detecting device: UV-detector; Detect wavelength: 550nm.
Embodiment 5
Take by weighing 2g water base adhesive sample, add 150mL water and be dissolved in the 250mL triangular flask, ultrasonic 15min is through the centrifugal 20min of hydro-extractor.Getting the 1mL supernatant liquor adds in the triangular flask, according to method preparation water base adhesive sample solution described above, with standard solution obtained above injection liquid chromatography behind 0.45 μ m filtering with microporous membrane, according to the determined method of the present invention, under chromatographic condition as described below, measure.
It is good that the result demonstrates the peak, and the chromatographic peak of boric acid separates fully with other component chromatographic peaks.
Wherein, chromatographic column: ZORBAX ODS; Mobile phase: methyl alcohol: water (50: 50 volume ratios); Chromatographic column temperature: 25 ℃; Sample size: 15 μ L; Flow velocity: 0.2mL/min; Detecting device: UV-detector; Detect wavelength: 550nm.
Claims (6)
1. the high performance liquid chromatography method for quantitatively determining of a water base adhesive mesoboric acid is characterized in that the method may further comprise the steps:
(1) take by weighing the water base adhesive sample, adding water is dissolved in and obtains solution in the triangular flask, then ultrasonic or vibration, centrifugal;
(2) get in the supernatant liquor adding triangular flask of mentioned solution, in triangular flask, add chromogenic reagent solution, mix afterwards evaporate to dryness on water-bath; Add solvent and be transferred in the volumetric flask, with solvent dilution to scale, mixing;
(3) solution liquid adopts high performance liquid chromatograph to analyze;
(4) adopt the relation of peak area and concentration direct ratio quantitative with external standard method.
2. the high performance liquid chromatography method for quantitatively determining of water base adhesive mesoboric acid according to claim 1, it is characterized in that: the sample weighting amount of the water base adhesive sample of described step (1) is 0.1-2g; The volume that adds entry is 10-1000mL, ultrasonic or duration of oscillation 10-30min; Centrifuge speed 4000-12000 turns; Centrifugation time is 5-30min.
3. the high performance liquid chromatography method for quantitatively determining of water base adhesive mesoboric acid according to claim 1 is characterized in that, the middle solution of described step (2) at the middle and upper levels clear liquid is got 0.1-2mL; Chromogenic reagent solution is the curcumin oxalic acid solution, and the consumption of developer is 2-8mL.
4. the high performance liquid chromatography method for quantitatively determining of water base adhesive mesoboric acid according to claim 1 is characterized in that, described step (2) water-bath temperature is the 30-60 degree, and the volumetric flask volume is 20-100mL.
5. the high performance liquid chromatography method for quantitatively determining of water base adhesive mesoboric acid according to claim 1 is characterized in that, in the described step (2) solvent be in methyl alcohol, 95% ethanol or the absolute ethyl alcohol any one.
6. the high performance liquid chromatography method for quantitatively determining of water base adhesive mesoboric acid according to claim 1, it is characterized in that, described step (3) chromatographic column adopting reverse-phase chromatographic column, mobile phase ratio: methyl alcohol: water=10-90: 90-10, chromatographic column column temperature: 20-35 ℃; The high performance liquid chromatography coutroi velocity is at 0.2～1mL/min; The employing UV-detector detects, and detects wavelength: 500-600nm.
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| CN103175787A (en) * | 2013-02-02 | 2013-06-26 | 广西中烟工业有限责任公司 | Method for measuring continuous flow ofboric acid in cigarette water-based glue |
| CN103487523A (en) * | 2013-09-24 | 2014-01-01 | 广西中烟工业有限责任公司 | Quantitative determination method for methylisothiazolinone and chloro methyl isothiazolinone in water-based adhesive |
| CN106442749A (en) * | 2016-07-14 | 2017-02-22 | 北京雷力海洋生物新产业股份有限公司 | Brown algae and detection method for detecting alginic acid content of brown algae product |
| CN113933404A (en) * | 2021-08-30 | 2022-01-14 | 北京泰德制药股份有限公司 | Method for measuring boric acid content |
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| CN103487523B (en) * | 2013-09-24 | 2014-12-03 | 广西中烟工业有限责任公司 | Quantitative determination method for methylisothiazolinone and chloro methyl isothiazolinone in water-based adhesive |
| CN106442749A (en) * | 2016-07-14 | 2017-02-22 | 北京雷力海洋生物新产业股份有限公司 | Brown algae and detection method for detecting alginic acid content of brown algae product |
| CN113933404A (en) * | 2021-08-30 | 2022-01-14 | 北京泰德制药股份有限公司 | Method for measuring boric acid content |
| CN113933404B (en) * | 2021-08-30 | 2023-05-05 | 北京泰德制药股份有限公司 | Method for measuring boric acid content |
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