CN102331470A - Method for determining content of bisphenol A in solution filled in feeding bottle - Google Patents
Method for determining content of bisphenol A in solution filled in feeding bottle Download PDFInfo
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- CN102331470A CN102331470A CN201110230426A CN201110230426A CN102331470A CN 102331470 A CN102331470 A CN 102331470A CN 201110230426 A CN201110230426 A CN 201110230426A CN 201110230426 A CN201110230426 A CN 201110230426A CN 102331470 A CN102331470 A CN 102331470A
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Abstract
The invention provides a method for determining content of bisphenol A in a solution filled in a feeding bottle. The method comprises the following steps of: A, determining test conditions of the method, selecting a chromatographic column according to retention characteristics of bisphenol A in a chromatograph, and making a corresponding chromatographic analysis method; B, making a standard curve for the relation of bisphenol A peak area and bisphenol A solution concentration; C, putting a food simulated aqueous solution into the feeding bottle, placing for 24 hours under the condition of water bath with the temperature of 40 DEG C, and preparing the solution filled in the feeding bottle; and D, testing the prepared solution filled in the feeding bottle according to the conditions determined in the step A, and thus obtaining the content of the bisphenol A in the solution filled in the feeding bottle. The method has the advantages of low using amount of samples, high detection sensitivity, high detection speed, high selectivity, and wide application range. Constant boiling point mixtures and materials with similar boiling points can be separated and analyzed by adopting the method.
Description
Technical field
the present invention relates to the assay method of content of bisphenol A in a kind of feeding bottle splendid attire solution.
Background technology
bisphenol-A is called for short bis-phenol base propane, is mainly used in macromolecular materials such as producing polycarbonate (PC), epoxy resin, polysulfone resin, polyphenylene oxide resin.Be widely used in aspects such as packaging material for food, container inner wall coating.Bisphenol-A is newfound a kind of incretion interferent from packaging material for food in recent years, can influence children's developmental process, particularly developmental fetus, baby and children.In October, 2008, federal government of canada announces: bisphenol-A is listed in the noxious material tabulation.Canada also becomes first bisphenol-A is regarded as the country of noxious material, and forbids in the manufacturing process of baby bottles, using bisphenol-A.European Union announces to forbid producing the plastics feeding bottle that contains bisphenol-A from March 1st, 2011, rises June and forbids that the import of any bisphenol-A plastics feeding bottle is to member state.In Chinese on May 30th, 2011,6 departments such as the Ministry of Public Health externally issue bulletin and claim, in view of the infant belongs to responsive crowd, are to take precautions against food safety risk, protect infantile health, forbid that bisphenol-A is used for infant feeding bottle.
are present; Mostly pertinent literature is environmental sample or aqueous sample for the analysis matrix of bisphenol-A, and detection method commonly used is a vapor-phase chromatography, but vapor-phase chromatography need be carried out acidylate, alkaneization, silanization etc. and derived; Operate more loaded down with trivial detailsly, detection efficiency is low.Therefore how to carry out to effective and rapid the content of bisphenol-A in the feeding bottle splendid attire solution, become the chemical analysis field problem demanding prompt solution.
Summary of the invention
For the vapor-phase chromatography that solves the prior art scheme is carried out content of bisphenol A analysis procedure complicacy in the solution, inefficient problem, the present invention provides following technical scheme:
The assay method of content of bisphenol A in a kind of feeding bottle splendid attire solution, this assay method may further comprise the steps:
A, confirm the test condition of this method, according to bisphenol-A retention characteristic in chromatogram, choose chromatographic column, and formulate corresponding red, orange, green, blue, yellow (ROGBY);
The typical curve of the relation of B, formulation bisphenol-A peak area and bisphenol-A solution concentration;
C, get food Simulated Water solution to feeding bottle,, produce feeding bottle splendid attire solution 40 ℃ of water bath condition held 24 hours;
D, the feeding bottle splendid attire solution of producing is tested according to the condition of confirming in the steps A, and drawn the content of bisphenol-A in the feeding bottle splendid attire solution.
As a kind of preferred version of the present invention, the test condition of confirming in the said steps A is:
Liquid-phase chromatographic column: C18 250 * 4.6mm, 5 μ m;
Column temperature: 30 ℃;
Moving phase: A acetonitrile, B water;
Gradient condition: 0～8min 50%A～68%A, 8～10min 68%A～50%A, 10～13min 50%A;
Flow velocity: 1.0mL/min;
fluorescence detector: excitation wavelength 230nm, emission wavelength 296nm.
As another kind of preferred version of the present invention, the method for drafting of said step B typical curve is following: accurately take by weighing bisphenol-A standard items 50mg, with dissolve with methanol and be settled to 50mL; Obtaining mass concentration is the bisphenol-A standard reserving solution of 1mg/mL; Get 5 parts of standard bisphenol-A storing solutions, be diluted to 0.05mg/mL, 0.1mg/mL, 0.2mg/mL, 0.4mg/mL, 0.5mg/mL with methyl alcohol respectively, the bisphenol-A after the dilution is tested under the test condition that steps A is set respectively; Concentration with bisphenol-A is horizontal ordinate; With the bisphenol-A peak area is that ordinate is made curve, obtains the typical curve of the relation of bisphenol-A peak area and bisphenol-A solution concentration, and funtcional relationship is Y=1 * 10
7
X+198012 obtains coefficient R
2
=0.9990.
as another preferred version of the present invention, solution uses the filter membrane of 0.45 μ m to filter earlier, and then detects before testing among the said step D.
The present invention has following advantage:
1, the inventive method amount of samples is few, and detection sensitivity is high, and detection speed is fast;
2, the inventive method selectivity is good, separable, analysis constant boiling mixture, the material that boiling point is close;
3, the inventive method applied range.
Description of drawings
The typical curve that
Fig. 1 the inventive method obtains.
Embodiment
are done to set forth in detail in the face of this process implementing example down, thereby so that advantage of the present invention and characteristic can be easier to it will be appreciated by those skilled in the art that protection scope of the present invention are made more explicit defining.
The assay method of content of bisphenol A in a kind of feeding bottle splendid attire solution, this assay method may further comprise the steps:
A, confirm the test condition of this method, according to bisphenol-A retention characteristic in chromatogram, choose chromatographic column, and formulate corresponding red, orange, green, blue, yellow (ROGBY); Test condition is following:
Liquid-phase chromatographic column: C18 250 * 4.6mm, 5 μ m;
Column temperature: 30 ℃;
Moving phase: A acetonitrile, B water;
Gradient condition: 0～8min 50%A～68%A, 8～10min 68%A～50%A, 10～13min 50%A;
Flow velocity: 1.0mL/min;
Fluorescence detector: excitation wavelength 230nm, emission wavelength 296nm;
The typical curve of the relation of B, formulation bisphenol-A peak area and bisphenol-A solution concentration; Concrete grammar is following: accurately take by weighing bisphenol-A standard items 50mg; With dissolve with methanol and be settled to 50mL, obtaining mass concentration is the bisphenol-A standard reserving solution of 1mg/mL, gets 5 parts of standard bisphenol-A storing solutions; Be diluted to 0.05mg/mL, 0.1mg/mL, 0.2mg/mL, 0.4mg/mL, 0.5mg/mL with methyl alcohol respectively; Bisphenol-A after the dilution is tested under the test condition that steps A is set respectively, is horizontal ordinate with the concentration of bisphenol-A, is that ordinate is made curve with the bisphenol-A peak area; Obtain the typical curve of the relation of bisphenol-A peak area and bisphenol-A solution concentration, funtcional relationship is Y=1 * 10
7
X+198012 obtains coefficient R
2
=0.9990, canonical plotting is as shown in Figure 1, and this typical curve is linear good;
C, get food Simulated Water solution to feeding bottle,, produce feeding bottle splendid attire solution 40 ℃ of water bath condition held 24 hours;
D, get three feeding bottles and do parallel appearance, be respectively parallel appearance 1, parallel appearance 2 is tested according to the condition of confirming in the steps A with parallel appearance 3, and the content that draws bisphenol-A in the feeding bottle splendid attire solution is shown in table one;
The content of bisphenol-A in the table one feeding bottle solution
To parallel appearance 1 replication 6 times, analysis result is seen table two,
The parallel appearance of table two 1 replication result
| Numbering | 1 | 2 | 3 | 4 | 5 | 6 | Mean value | RSD（%） |
| BPA concentration (mg/L) | 0.025 | 0.024 | 0.024 | 0.025 | 0.026 | 0.023 | 0.025 | 4.28% |
Learn through analysis
, and the relative standard deviation of replication experiment is 4.28%, good reproducibility.According to the detection method of step of the present invention, its method recovery of standard addition of side, the result is as shown in table 3,
Table three determination of recovery rates
| Sample content (mg/L) | Addition (mg/L) | Measured value (mg/L) | The recovery (%) |
| 0 | 0.050 | 0.041 | 82% |
| 0 | 0.100 | 0.090 | 90% |
| 0 | 0.200 | 0.187 | 93.5% |
mat can see that in above-mentioned testing result the method detectability that detection method of the present invention detects bisphenol-A in the feeding bottle solution is low, highly sensitive, and detection speed is fast, can carry out detection by quantitative to bisphenol-A in the feeding bottle accurately.
the above; Be merely one of embodiment of the present invention; But protection scope of the present invention is not limited thereto; Any those of ordinary skill in the art are in the technical scope that the present invention disclosed, and variation or the replacement that can expect without creative work all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims were limited.
Claims (4)
1. the assay method of content of bisphenol A in the feeding bottle splendid attire solution, it is characterized in that: this assay method may further comprise the steps:
A, confirm the test condition of this method, according to bisphenol-A retention characteristic in chromatogram, choose chromatographic column, and formulate corresponding red, orange, green, blue, yellow (ROGBY);
The typical curve of the relation of B, formulation bisphenol-A peak area and bisphenol-A solution concentration;
C, get food Simulated Water solution to feeding bottle,, produce feeding bottle splendid attire solution 40 ℃ of water bath condition held 24 hours;
D, the feeding bottle splendid attire solution of producing is tested according to the condition of confirming in the steps A, and drawn the content of bisphenol-A in the feeding bottle splendid attire solution.
2. the assay method of content of bisphenol A in a kind of feeding bottle splendid attire solution according to claim 1 is characterized in that: the test condition of confirming in the said steps A is:
Liquid-phase chromatographic column: C18 250 * 4.6mm, 5 μ m;
Column temperature: 30 ℃;
Moving phase: A acetonitrile, B water;
Gradient condition: 0～8min 50%A～68%A, 8～10min 68%A～50%A, 10～13min 50%A;
Flow velocity: 1.0mL/min;
Fluorescence detector: excitation wavelength 230nm, emission wavelength 296nm.
3. the assay method of content of bisphenol A in a kind of feeding bottle splendid attire solution according to claim 1; It is characterized in that: the method for drafting of said step B typical curve is following: accurately take by weighing bisphenol-A standard items 50mg; With dissolve with methanol and be settled to 50mL, obtaining mass concentration is the bisphenol-A standard reserving solution of 1mg/mL, gets 5 parts of standard bisphenol-A storing solutions; Be diluted to 0.05mg/mL, 0.1mg/mL, 0.2mg/mL, 0.4mg/mL, 0.5mg/mL with methyl alcohol respectively; Bisphenol-A after the dilution is tested under the test condition that steps A is set respectively, is horizontal ordinate with the concentration of bisphenol-A, is that ordinate is made curve with the bisphenol-A peak area; Obtain the typical curve of the relation of bisphenol-A peak area and bisphenol-A solution concentration, funtcional relationship is Y=1 * 10
7X+198012 obtains coefficient R
2=0.9990.
4. the assay method of content of bisphenol A in a kind of feeding bottle splendid attire solution according to claim 1 is characterized in that: solution uses the filter membrane of 0.45 μ m to filter earlier, and then detects before testing among the said step D.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110230426A CN102331470A (en) | 2011-08-11 | 2011-08-11 | Method for determining content of bisphenol A in solution filled in feeding bottle |
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| CN201110230426A CN102331470A (en) | 2011-08-11 | 2011-08-11 | Method for determining content of bisphenol A in solution filled in feeding bottle |
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| CN102331470A true CN102331470A (en) | 2012-01-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590429A (en) * | 2012-02-29 | 2012-07-18 | 广州市质量监督检测研究院 | Method for determining content of additive for food packaging material |
| CN106290691A (en) * | 2016-11-01 | 2017-01-04 | 中国检验检疫科学研究院 | The fast quantitative measurement method for detecting of bisphenol compound in a kind of milk product |
| CN110887903A (en) * | 2018-09-11 | 2020-03-17 | 山东省医疗器械产品质量检验中心 | Method for measuring bisphenol A residue in hemodialyzer |
-
2011
- 2011-08-11 CN CN201110230426A patent/CN102331470A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 冼燕萍等: "奶瓶中双酚A、烷基酚及烷基酚聚氧乙烯醚残留量的高效液相色谱-荧光测定法", 《现代食品科技》 * |
| 郭春海等: "聚碳酸酯奶瓶中双酚A单体向食品模拟物迁移规律的研究", 《食品科学》 * |
| 陈志锋等: "食品接触材料中双酚类物质迁移检测方法研究", 《包装工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590429A (en) * | 2012-02-29 | 2012-07-18 | 广州市质量监督检测研究院 | Method for determining content of additive for food packaging material |
| CN102590429B (en) * | 2012-02-29 | 2014-07-09 | 广州市质量监督检测研究院 | Method for determining content of additive for food packaging material |
| CN106290691A (en) * | 2016-11-01 | 2017-01-04 | 中国检验检疫科学研究院 | The fast quantitative measurement method for detecting of bisphenol compound in a kind of milk product |
| CN110887903A (en) * | 2018-09-11 | 2020-03-17 | 山东省医疗器械产品质量检验中心 | Method for measuring bisphenol A residue in hemodialyzer |
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Application publication date: 20120125 |