CN109932457A - A kind of method of denatonium benzoate content in detection toy material - Google Patents
A kind of method of denatonium benzoate content in detection toy material Download PDFInfo
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- CN109932457A CN109932457A CN201910309855.5A CN201910309855A CN109932457A CN 109932457 A CN109932457 A CN 109932457A CN 201910309855 A CN201910309855 A CN 201910309855A CN 109932457 A CN109932457 A CN 109932457A
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Abstract
The invention discloses a kind of methods of denatonium benzoate content in detection toy material, including preparing Standard Stock solutions respectively, intermediate Working Standard Solution and series of concentrations standard solution, sample to be tested is pre-processed, carry out high performance liquid chromatography detection, using acetonitrile-water (30:70, v/v) solution is as Extraction solvent, through ultrasonic extraction, constant volume, after filtering, gradient elution is carried out by mobile phase of acetonitrile-water, use C-18 column for chromatographic column, with photodiode array detector, denatonium benzoate Detection wavelength is 227.4nm, detection is limited to 2.66ng (in terms of 3 times of signal-to-noise ratio), average recovery rate is 99.3%, method precision is 0.81%~2.36%.This method detection limit is low, precision is high; it is suitble to the measurement of the field bitters denatonium benzoate content; to China's liquid or sticky toy improvement level is promoted, the legitimate rights and interests of Chinese children consumer are protected, while having great importance to the smooth outlet for promoting China's toy product.
Description
Technical field
The invention belongs to technical field of analytical chemistry, are related to a kind of side for detecting denatonium benzoate content in toy material
Method, bitters denatonium benzoate assay high performance liquid chromatography in specially a kind of liquid or sticky toy material.
Background technique
Liquid or sticky type toy, such as moulding loam, to point at pigment passed through for the specially designed type toy of children
It is dipped with hand or finger and carries out moulding or drawing use.Children's autocontrol force is poor, and health consciousness is weak, and children are using and playing
It is careless slightly when playing this type toy, oral cavity is touched by finger, the poisonous and harmful substance in this type toy can enter its body
It is interior, the physical and mental health of children is caused to seriously endanger.Therefore countries in the world launch respectively stringent rule and standard to liquid or
Bitters is limited to inhibit children to eat by mistake in sticky type toy.
Bitters also known as hinders food agent, is that one kind makes an addition in product, its taste or smell is made to have the chemicals of bitter taste,
Be it is a kind of for prevent people suck or intake poisonous and harmful substance (such as methanol, industrial alcohol and ethylene glycol) and widely used detest
Dislike agent.Denatonium benzoate is also referred to as bitter, and structure is made of two parts of benzoic acid group and denatonium group.It is currently known
Most bitter compound, be the Typical Representative of bitter compounds, bitter taste is 1000 times of quinine hardship degree.Due to denatonium benzoate
Only need minute quantity addition that can play resistance food effect, so requiring the bitters of addition in liquid or sticky type toy usually thus
This compound.
Currently, there is no the detection method of bitters denatonium benzoate in liquid or sticky type toy both at home and abroad.Also not yet
See the detection document report of related denatonium benzoate.
Summary of the invention
The purpose of the present invention is intended to provide bitters denatonium benzoate content in a kind of liquid or sticky type toy material
The high performance liquid chromatography of detection simultaneously solves difficulty of the domestic and international field without bitters denatonium benzoate detection method
Topic.
The present invention is realized especially by following technical scheme:
A kind of method of denatonium benzoate content in detection toy material, including prepare respectively Standard Stock solutions, in
Between Working Standard Solution and series of concentrations standard solution, sample to be tested is pre-processed, carry out high performance liquid chromatography detection；
The testing conditions of the high performance liquid chromatography detection are as follows:
Chromatographic column: C-18 column；Flow velocity: 0.3mL/min；Detection wavelength: 227.4nm；Column temperature: 30 DEG C；Mobile phase: acetonitrile-
The following gradient elution of water:
| Time | Flow velocity mL/min | Acetonitrile (mobile phase A) | Ultrapure water (Mobile phase B) |
| 0 | 0.3 | 10 | 90 |
| 1 | 0.3 | 30 | 70 |
| 5 | 0.3 | 30 | 70 |
| 7 | 0.3 | 50 | 50 |
| 9 | 0.3 | 10 | 90 |
The preparation of the Standard Stock solutions: accurately weighing denatonium benzoate in small beaker, and suitable second is added
Nitrile-water (30:70, v/v) solution after ultrasonic dissolution, is settled to scale with acetonitrile-aqueous solution, shakes up, being made into mass concentration is about
The standard reserving solution of 1000mg/L；
The preparation of the intermediate Working Standard Solution: Standard Stock solutions are pipetted into volumetric flask, use acetonitrile-aqueous solution
Constant volume shakes up, and is made into the intermediate Working Standard Solution that mass concentration is about 50mg/L；
The series of concentrations standard solution: intermediate working stamndard 0.20,1.00,20.00,10.0mL solution and mark are pipetted
Quasi- stock solution 1.00,2.50,5.00,10.00mL are placed in volumetric flask, are shaken up with acetonitrile-water dilution, obtain mass concentration
The respectively standard solution of 1mg/L, 5mg/L, 10mg/L, 50mg/L, 100mg/L, 250mg/L, 500mg/L and 1000mg/L；
The sample pretreatment: weighing sample in color-comparison tube, is added extractant acetonitrile-water (30:70, v/v)
Solution, and sealed with sealed membrane, through vortex shaking and ultrasonic extraction, membrane filtration, filtrate is spare as the sample solution to be tested.
The invention has the benefit that
1) operation of the present invention is easy.Using acetonitrile-water (30:70, v/v) solution, as Extraction solvent, through ultrasonic extraction
20min, constant volume after filtering, carry out gradient elution by mobile phase of acetonitrile-water, use C-18 column for chromatographic column, with two pole of photoelectricity
Pipe array (PDA) detector, denatonium benzoate Detection wavelength are 227.4nm.
2) method accuracy height, favorable reproducibility.The detection of denatonium benzoate method limits (in terms of 3 times of signal-to-noise ratio)
2.66ng, within the scope of (1.000~1000) mg/L, peak area and mass concentration are in good linear relationship, and related coefficient is
0.9997.Average recovery rate is 99.3%, and relative standard deviation is 0.81%~2.63%.
Specific embodiment
Below in conjunction with specific embodiment of the present invention, technical solution of the present invention is clearly and completely described, is shown
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
The present invention provides it is a kind of detection toy material in denatonium benzoate content method, using acetonitrile-water (30:
70, v/v) solution is as Extraction solvent, and through ultrasonic extraction 20min, constant volume after filtering, carries out gradient by mobile phase of acetonitrile-water
Elution, uses C-18 column for chromatographic column, with photodiode array (PDA) detector, denatonium benzoate Detection wavelength is
227.4nm.Specific step is as follows:
1) instrument and reagent
Waters H-class ultra performance liquid chromatography (Waters, US) is furnished with diode array detector
(DAD) and autosampler；Ultrasonic cleaner (Branson company), a ten thousandth electronic analytical balance (Beijing Sai Duolisi
Co., Ltd), Milli-Q Intergral water purification machine (French Millipore company), denatonium benzoate (purity
99.5%), acetonitrile (chromatographically pure, Fisher company)；Ultrapure water (18.2M Ω cm).
2) preparation of standard solution
Standard Stock solutions (1000mg/L): denatonium benzoate 0.05g (being accurate to 0.0001g) is accurately weighed in small burning
In cup, suitable acetonitrile-water (30:70, v/v) solution is added, is transferred in the volumetric flask of 50mL after ultrasonic dissolution, with acetonitrile-
Water (30:70, v/v) solution is settled to scale, shakes up, and is made into the standard reserving solution that mass concentration is about 1000mg/L.
Intermediate Working Standard Solution (50mg/L): the Standard Stock solutions 5.0mL of 1000mg/L is pipetted to 100mL volumetric flask
In, it is settled to scale with acetonitrile-water (30:70, v/v) solution, is shaken up, the intermediate work mark that mass concentration is about 50mg/L is made into
Quasi- solution.
Series of concentrations standard solution: pipette among denatonium benzoate working stamndard 0.20,1.00,20.00,10.0mL it is molten
Liquid and Standard Stock solutions 1.00,2.50,5.00,10.00mL are placed in 10mL volumetric flask, with acetonitrile-water (30:70, v/v)
It is diluted to scale, is shaken up, obtaining mass concentration is respectively 1.00,5.00,10.0,50.0,100,250,500 and 1000mg/L
Standard solution.
3) sample pretreatment
Sample about 1.0g (being accurate to 0.0001g) is weighed in 10mL color-comparison tube, extractant (acetonitrile-water is added
(30:70, v/v) solution is sealed to scale and with sealed membrane, vortex shaking 1min, ultrasonic extraction 20min, when necessary can high speed from
The heart.Through 0.22 μm of membrane filtration, filtrate is spare as the sample solution to be tested.
4) chromatographic condition
Chromatographic column: BEH C18Column (100mm × 2.1mm, 1.7 μm), mobile phase: acetonitrile-water presses 1 gradient elution of table；Flow velocity:
0.3mL/min；DAD Detection wavelength: 227.4nm；Column temperature: 30 DEG C；Sample volume: 1 μ L.
1 eluent gradient of table elutes table
| Time | Flow velocity mL/min | Acetonitrile (mobile phase A) | Ultrapure water (Mobile phase B) |
| 0 | 0.3 | 10 | 90 |
| 1 | 0.3 | 30 | 70 |
| 5 | 0.3 | 30 | 70 |
| 7 | 0.3 | 50 | 50 |
| 9 | 0.3 | 10 | 90 |
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understand without departing from the principles and spirit of the present invention can to these examples carry out it is a variety of variation, modification, replacement and
Modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of method of denatonium benzoate content in detection toy material characterized by comprising prepare standard storage respectively
Standby solution, intermediate Working Standard Solution and series of concentrations standard solution, sample to be tested is pre-processed, high-efficient liquid phase color is carried out
Spectrum detection；
The testing conditions of the high performance liquid chromatography detection are as follows:
Chromatographic column: C-18 column；Flow velocity: 0.3mL/min；Detection wavelength: 227.4nm；Column temperature: 30 DEG C；Mobile phase: acetonitrile-water is such as
Gradient elution:
2. the method for denatonium benzoate content in a kind of detection toy material according to claim 1, which is characterized in that
The preparation of the Standard Stock solutions: accurately weighing denatonium benzoate in small beaker, and it is molten that suitable acetonitrile-water is added
Liquid after ultrasonic dissolution, is settled to scale with acetonitrile-aqueous solution, shakes up, be made into the standard inventory that mass concentration is about 1000mg/L
Liquid.
3. the method for denatonium benzoate content in a kind of detection toy material according to claim 1, which is characterized in that
The preparation of the intermediate Working Standard Solution: pipetting Standard Stock solutions into volumetric flask, is shaken with acetonitrile-aqueous solution constant volume
It is even, it is made into the intermediate Working Standard Solution that mass concentration is about 50mg/L.
4. the method for denatonium benzoate content in a kind of detection toy material according to claim 1, which is characterized in that
The series of concentrations standard solution: it is molten that intermediate working stamndard 0.20,1.00,20.00,10.0mL solution and standard inventory are pipetted
Liquid 1.00,2.50,5.00,10.00mL are placed in volumetric flask, are shaken up with acetonitrile-water dilution, obtaining mass concentration is respectively
The standard solution of 1mg/L, 5mg/L, 10mg/L, 50mg/L, 100mg/L, 250mg/L, 500mg/L and 1000mg/L.
5. the method for denatonium benzoate content in a kind of detection toy material according to claim 1, which is characterized in that
The sample pretreatment: weighing sample in color-comparison tube, and extractant acetonitrile solution is added and is sealed with sealed membrane, through whirlpool
Rotation shaking and ultrasonic extraction, membrane filtration, filtrate are spare as the sample solution to be tested.
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| CN201910309855.5A CN109932457B (en) | 2019-04-17 | 2019-04-17 | Method for detecting content of denatonium benzoate in toy material |
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| CN201910309855.5A CN109932457B (en) | 2019-04-17 | 2019-04-17 | Method for detecting content of denatonium benzoate in toy material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110441416A (en) * | 2019-07-26 | 2019-11-12 | 上海海关机电产品检测技术中心 | A kind of method that ultra performance liquid chromatography measurement children point at bitters aurantiin and denatonium benzoate in ink paste |
| CN112526037A (en) * | 2020-12-07 | 2021-03-19 | 温州市质量技术检测科学研究院 | Method for detecting bitter essence in Bake balls |
Citations (1)
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| CN102297925A (en) * | 2007-02-01 | 2011-12-28 | 北京亚东生物制药有限公司 | Detection method of traditional Chinese medicine composition for treating kidney-yang deficiency |
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2019
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102297925A (en) * | 2007-02-01 | 2011-12-28 | 北京亚东生物制药有限公司 | Detection method of traditional Chinese medicine composition for treating kidney-yang deficiency |
Non-Patent Citations (4)
| Title |
|---|
| DAMON, CE 等: "HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC DETERMINATION OF DENATONIUM BENZOATE IN RAPESEED OIL", 《JOURNAL OF CHROMATOGRAPHY》 * |
| FAULKNER, A 等: "HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC DETERMINATION OF DENATONIUM BENZOATE IN ETHANOL WITH 5-PERCENT POLYVINYLPYRROLIDONE", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| GADZALA-KOPCIUCH 等: "Isolation and determination of denatonium benzoate in antifreezing agents by solid phase extraction and HPLC", 《GADZALA-KOPCIUCH 等》 * |
| MORI，NAKAMURA 等: "Determination of denatonium benzoate in cosmetics and their antifeeding property", 《化学生物総合管理》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110441416A (en) * | 2019-07-26 | 2019-11-12 | 上海海关机电产品检测技术中心 | A kind of method that ultra performance liquid chromatography measurement children point at bitters aurantiin and denatonium benzoate in ink paste |
| CN112526037A (en) * | 2020-12-07 | 2021-03-19 | 温州市质量技术检测科学研究院 | Method for detecting bitter essence in Bake balls |
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