CN108535370A - The detection method of phenolic compound in a kind of carbonic ester packaging material for food - Google Patents
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Abstract
The invention discloses a kind of detection methods of phenolic compound in carbonic ester packaging material for food, belong to packaging material technical field of analysis and detection, including having the following steps：1. preparing standard solution；2. liquid phase chromatogram condition optimizes；3. Mass Spectrometry Conditions optimize；4. the range of linearity and detection limit measure；5. sample pre-treatments；6. sample detection.The detection method establishes high performance liquid chromatography tandem mass spectrum while measuring the quantitative analysis method of nonyl phenol, octyl phenol, p -cumylphenol and bisphenol-A in makrolon material food contact material, quickly, accurately, high sensitivity, and pre-treatment step is simple, the raw material that contact material class manufacturing enterprise is met for the vast food in China is checked on and final product quality control provides simple and reliable analysis method.
Description
Technical field
The present invention relates to packaging material technical field of analysis and detection, in particular to phenol in a kind of carbonic ester packaging material for food
The detection method of class compound.
Background technology
In food contact material, makrolon（Polycarbonate,PC）Resin because its with the excellent transparency,
The performances such as dimensional stability, impact resistance are widely used in baby bottles, Space cup, plastic tableware and beverage bottle, drinking water
In the manufacturings of containers such as bucket.
Phenolic compound is the key industry original for producing the high molecular materials such as epoxy resin, makrolon and polysulfone resin
Material.Studies have shown that phenolic compound is mainly bisphenol-A in polycarbonate food contact material（BPA）, p -cumylphenol（CP）、
Nonyl phenol（NP）, octyl phenol（OP）4 kinds.Olso-Paris Convention（OSPAR）Also nonyl phenol and octyl phenol are included in preferential control
Polluter register processed.The U.S., Canada, European Union and the Chinese application for being prevented or restricted from bisphenol-A on articles for children of having made laws.
Chinese food is packed for makrolon（PC）Sanitary standard in define the limitation of phenol in resin material and molded product and be
0.05mg/L。
Currently, the detection method for above-mentioned 4 kinds of phenolic compounds mainly has high performance liquid chromatography, liquid chromatogram-string
Join mass spectrography, capillary electrophoresis, gas chromatography-mass spectrography, enzyme linked immunosorbent assay analysis method etc..However these methods detect
Phenolic compound type it is limited, detected while cannot be satisfied major phenolic compound in polycarbonate food contact material
Demand.
Invention content
In view of the above technical problems, the present invention is using above-mentioned 4 kinds of phenolic compounds as object, extracting method, color to sample
The expansion such as spectral condition, Mass Spectrometry Conditions are studied.By screening and optimizing, propose above-mentioned suitable for polycarbonate food contact material
The pre-treating method of 4 kinds of phenolic compounds establishes while detecting in polycarbonate food contact material 4 kinds of phenolic compounds
HPLC-MS/MS methods, to establish method with assessment for the Risk Monitoring of polycarbonate food contact material phenolic compound
Basis.
To achieve the above object, the present invention designed by a kind of carbonic ester packaging material for food in phenolic compound detection
Method, including having the following steps：
1. preparing standard solution：The standard items of target components are subjected to constant volume using methanol, are configured to the standard of a fixed concentration
Solution；
2. liquid phase chromatogram condition optimizes：Set liquid phase chromatogram condition to following parameter：
Using ZORBAX Extend C18 chromatographic columns, specification 50mm*2.1mm, 3.5 μm；Column temperature is set as 35 DEG C；Flow velocity
For 0.2mL/min；Sampling volume is 5 μ L；
3. Mass Spectrometry Conditions optimize：Set Mass Spectrometry Conditions to following parameter：
Using electric spray ion source；Scan mode is negative ion mode；Capillary voltage is 3.50kV；Detection mode is mostly anti-
It should monitor；Ion source temperature is 100 DEG C；It is 300 DEG C to remove solvent temperature degree；
Mass spectrum multiple-reaction monitoring technology（MRM）It is one kind based on Given information or assumes that information targetedly obtains data, into
The technology of row mass signal acquisition, it is sensitive, accurate and special to have many advantages, such as.It is based on reactive ion letter that is known or assuming
Breath, targetedly selects data and carries out mass signal acquisition, carries out signal record to legal ion, removal is not met
The interference of regular ion signal, by the statistical analysis to data to obtain the mass-spectrometric technique of mass spectrum quantitative information.MRM technologies
It is to develop on the basis of single reaction monitoring technology.Key is to first have to be able to detect that for MRM technologies
Then selected specific parent ion is only carried out collision-induced, finally removes other daughter ions by the parent ion with specificity
Interference, the acquisition of mass signal is only carried out to selected special daughter ion.Since triple level four bars mass spectrums are to carry out single matter
Lotus is the mass spectrometer for being most suitable for MRM analyses than scanning most sensitive mass spectrometer system；
4. the range of linearity and detection limit measure：Investigate linear relationship and correlation of the target components in 0.2 ~ 2mg/L concentration ranges
The inspection of corresponding a concentration of the method when coefficient, and add in blank sample the target components of various concentration with signal-to-noise ratio is 3
Rising limit, signal-to-noise ratio corresponding a concentration of lower limit of quantitation when being 10；
Signal-to-noise ratio, English name are called SNR or S/N（SIGNAL-NOISE RATIO), also known as signal to noise ratio refers to an electronics
The ratio of signal and noise in equipment or electronic system；
5. sample pre-treatments：By sample by being manually crushed, then by beveller it is crushed, then uses dichloromethane
It is extracted under ultrasound condition to crushing sample, methanol dissolved residue is used after extracting solution drying, it is to be determined after filtering；
6. sample detection：High performance liquid chromatography-tandem mass instrument after being optimized using above-mentioned condition is detected sample.
As a preferred embodiment of the above technical solution, 1. the target components are bisphenol-A, nonyl phenol, octyl phenol and to withered to step
Base phenol.
As a preferred embodiment of the above technical solution, 1. step weighs 1mg target components in 10ml volumetric flasks, is carried out with methanol
Constant volume is made into the standard solution of 100mg/L, is then stored in the environment of -20 DEG C.
As a preferred embodiment of the above technical solution, step 5. in sample is cut by block using scissors first, then use
Liquid nitrogen is freezed, then crushing is ground to it using freeze grinding instrument.
As a preferred embodiment of the above technical solution, step 5. in weigh 2.0g after sample comminution and be placed in tool plug test tube, be added
10ml dichloromethane, ultrasonic extraction 1 hour under 30 ~ 50 degrees celsius, extracting solution is concentrated with Rotary Evaporators, nitrogen drying
Afterwards, 1mL methanol dissolved residues are added, are filtered with 0.20 μm of miillpore filter rear to be determined.
As a preferred embodiment of the above technical solution, step 5. in step 5. in weigh 2.0g after sample comminution and be placed in tool plug test tube
In, 10ml dichloromethane is added, ultrasonic extraction 1 hour under 40 degrees celsius, extracting solution is concentrated with Rotary Evaporators, nitrogen
After drying, 1mL methanol dissolved residues are added, are filtered with 0.20 μm of miillpore filter rear to be determined.
As a preferred embodiment of the above technical solution, step 2. in liquid chromatogram mobile phase be A- methanol, B-0.1% ammonium hydroxide.
The substance that component to be measured moves forward is carried in chromatographic process and is known as mobile phase, and equilibrium-like is in stationary phase
State simultaneously drives sample to move forward, and herein described mobile phase is made of methanol and 0.1% ammonium hydroxide compounding.
As a preferred embodiment of the above technical solution, step 2. in gradient elution program be that 0 ~ 2min corresponds to the stream of 80%A-20%B
Dynamic phase, 2 ~ 6min correspond to the mobile phase of 60%A-40%B, 6 ~ 12min corresponds to the mobile phase of 80%A-20%B.
Aforementioned proportion is mass ratio.
Gradient elution is also known as gradient elution or program elution, i.e., in the same analytical cycle, by a certain degree constantly
The concentration proportioning for changing mobile phase, the method for then using gradient elution to the sample of complicated components in liquid chromatogram, can make
The larger component of nature difference in one complex sample can reach good separation purpose by respectively suitable capacity factor measure k.
As a preferred embodiment of the above technical solution, step 3. in go the solvent gas and taper hole gas to be high pure nitrogen, flow velocity difference
For 500L/h and 50L/h.
As a preferred embodiment of the above technical solution, 3. middle collision gas is high-purity argon gas to step.
When using argon gas as collision gas, low quality number cut-off effect can be effectively improved and improve ion collision process
In energy transfer efficiency, while improving ion trap and dissociation efficiency, but mass resolution can be substantially reduced.
Compared with prior art, the present invention haing the following advantages and advantageous effect：
The present invention establishes high performance liquid chromatography-tandem mass while measuring nonyl in makrolon material food contact material
The quantitative analysis method of phenol, octyl phenol, p -cumylphenol and bisphenol-A.This method quickly, accurate, high sensitivity, pre-treatment step
Simply, it disclosure satisfy that vast base's packaging material for food examines the needs in laboratory, also connect contact material for the vast food in China
The raw material of class manufacturing enterprise is checked on and final product quality control provides simple and reliable analysis method.
Description of the drawings
The MRM chromatograms of target components when Fig. 1 is using -0.1% ammonia spirit of methanol as mobile phase.
Specific implementation mode
The present invention is described in further detail in the following with reference to the drawings and specific embodiments：
Embodiment：20 PC scuttlebutts, 5 PC feeding bottles and 5 PC are drunk respectively using detection method of the present invention
The bisphenol-A contained in cup（BPA）, nonyl phenol（NP）, octyl phenol（OP）And p -cumylphenol（CP）It is detected.
The reagent of use and instrument are as follows：
Reagent：Bisphenol-A, nonyl phenol, octyl phenol, p -cumylphenol standard items（Purity 99%, German Dr.Ehrenstorfer standards
Product）, methanol（Chromatographically pure, Shanghai Aladdin reagent）, other reagents are that analysis is pure, and experimental water is ultra-pure water；
Instrument：1260/6430 high performance liquid chromatography-tandem mass instrument（HPLC-MS/MS, Agilent companies of the U.S.）, Milli-Q
Superpure water machine（Millipore companies of the U.S.）, Retsch ZM200 freeze grinding instrument（German Retsch companies）, the rotations of RV 10
Evaporimeter（German IKA）, electronic analytical balance（Accuracy 0.0001mg）.
Detection method is as follows：
1. preparing standard solution：The standard items of bisphenol-A, nonyl phenol, octyl phenol and p -cumylphenol are weighed 1mg respectively to be placed in
In 10ml volumetric flasks, constant volume is carried out with methanol, is made into the standard solution of 100mg/L, is then stored in -20 DEG C of environment
Under；
2. liquid phase chromatogram condition optimizes：Set liquid phase chromatogram condition to following parameter：
Using ZORBAX Extend C18 chromatographic columns, specification 50mm*2.1mm, 3.5 μm；Column temperature is set as 35 DEG C；Flow velocity
For 0.2mL/min；Sampling volume is 5 μ L；Mobile phase is A- methanol, B-0.1% ammonium hydroxide；Gradient elution program corresponds to for 0 ~ 2min
The mobile phase of 80%A-20%B, 2 ~ 6min correspond to the mobile phase of 60%A-40%B, 6 ~ 12min corresponds to the mobile phase of 80%A-20%B；
3. Mass Spectrometry Conditions optimize：Set Mass Spectrometry Conditions to following parameter：
Using electric spray ion source；Scan mode is negative ion mode；Capillary voltage is 3.50kV；Detection mode is mostly anti-
It should monitor；Ion source temperature is 100 DEG C；It is 300 DEG C to remove solvent temperature degree；It is high pure nitrogen to remove solvent gas and taper hole gas, stream
Speed is respectively 500L/h and 50L/h；Collision gas is high-purity argon gas；
4. the range of linearity and detection limit measure：Investigate linear relationship and correlation of the target components in 0.2 ~ 2mg/L concentration ranges
The inspection of corresponding a concentration of the method when coefficient, and add in blank sample the target components of various concentration with signal-to-noise ratio is 3
Rising limit, signal-to-noise ratio corresponding a concentration of lower limit of quantitation when being 10；
5. sample pre-treatments：Sample is cut by block using scissors first, is then freezed using liquid nitrogen, then using freezing
Beveller is ground it crushing, and weighing 2.0g after sample comminution is placed in tool plug test tube, 10ml dichloromethane is added, 40 take the photograph
Ultrasonic extraction 1 hour under the conditions of family name's degree, extracting solution is concentrated with Rotary Evaporators, and after nitrogen drying, it is residual that the dissolving of 1mL methanol is added
Slag is filtered rear to be determined with 0.20 μm of miillpore filter；
6. sample detection：High performance liquid chromatography-tandem mass instrument after being optimized using above-mentioned condition is detected sample.
The tandem mass spectrum detection parameters of target components are shown in Table 1：
The tandem mass spectrum detection parameters of 1 target components of table
Totally 5 kinds of water phases and acetonitrile, 2 kinds of methanol have for comparative studies of the present invention 0.1% ammonium hydroxide, buffer salt, ammonium acetate, phosphoric acid and water
Machine mutually as mobile phase when 4 kinds of phenolic compounds separating effect.The result shows that using -0.1% ammonia spirit of methanol as flowing
The peak shape of Xiang Shi, 4 kinds of phenolic compounds are obviously improved, and obtain preferable separating effect and response, as shown in Figure 1.
Based on the chromatography-mass spectroscopy condition after optimization, investigated bisphenol-A, nonyl phenol, octyl phenol, p -cumylphenol 0.2 ~
Linear relationship in 2mg/L concentration ranges and related coefficient, and in blank sample add low concentration each target compound, with
Signal-to-noise ratio is 3（S/N=3）When corresponding a concentration of the method detection limit, the corresponding a concentration of lower limit of quantitation in S/N=10.As a result
Show that the linear relationship of bisphenol-A, nonyl phenol, octyl phenol, p -cumylphenol in 0.2 ~ 2mg/L concentration ranges is good.Phase relation
Number is not less than 0.9993, and linear equation, related coefficient, detection limit and quantitative limit are shown in Table 2.
2 linear relationship of table, detection limit and lower limit of quantitation
The mixed standard solution of basic, normal, high 3 concentration levels, each concentration parallel determination 5 times, meter are added into blank sample
Recovery of standard addition and relative standard deviation are calculated, table 3 is as a result listed in.The recovery of standard addition of mixed standard solution is 84.4%-108.8%
, relative standard deviation（RSD）For 1.0%-12.4%, this method shows higher accuracy and precision.
The rate of recovery and relative standard deviation of 3 standard solution of table（n=5）
20 PC scuttlebutts, 5 PC feeding bottles, 5 drinking water glass are detected using this method and amount to 30 samples.As a result it shows,
Detect that bisphenol-A, content detect nonyl in 40.78 μ g/kg-1752.69 μ g/kg, 13 samples in 30 samples
Phenol, content detect p -cumylphenol in 107.83 μ g/kg-145.22 μ g/kg, 5 samples, content 50.36 μ g/
Kg-384.4 μ g/kg, octyl phenol are not detected, and testing result is shown in Table 4：
4 kinds of content of phenolic compounds measure in 4 PC packaging materials for food of table
Claims (10)
1. the detection method of phenolic compound in a kind of carbonic ester packaging material for food, which is characterized in that comprising having the following steps：
1. preparing standard solution：The standard items of target components are subjected to constant volume using methanol, are configured to the standard of a fixed concentration
Solution；
2. liquid phase chromatogram condition optimizes：Set liquid phase chromatogram condition to following parameter：
Using ZORBAX Extend C18 chromatographic columns, specification is 50mm × 2.1mm, 3.5 μm；Column temperature is set as 35 DEG C；Flow velocity
For 0.2mL/min；Sampling volume is 5 μ L；
3. Mass Spectrometry Conditions optimize：Set Mass Spectrometry Conditions to following parameter：
Using electric spray ion source；Scan mode is negative ion mode；Capillary voltage is 3.50kV；Detection mode is mostly anti-
It should monitor；Ion source temperature is 100 DEG C；It is 300 DEG C to remove solvent temperature degree；
4. the range of linearity and detection limit measure：Investigate linear relationship and correlation of the target components in 0.2 ~ 2mg/L concentration ranges
The inspection of corresponding a concentration of the method when coefficient, and add in blank sample the target components of various concentration with signal-to-noise ratio is 3
Rising limit, signal-to-noise ratio corresponding a concentration of lower limit of quantitation when being 10；
5. sample pre-treatments：By sample by being manually crushed, then by beveller it is crushed, then uses dichloromethane
It is extracted under ultrasound condition to crushing sample, methanol dissolved residue is used after extracting solution drying, it is to be determined after filtering；
6. sample detection：High performance liquid chromatography-tandem mass instrument after being optimized using above-mentioned condition is detected sample.
2. the detection method of phenolic compound, feature in a kind of carbonic ester packaging material for food according to claim 1
It is：1. the target components are bisphenol-A, nonyl phenol, octyl phenol and p -cumylphenol to step.
3. the detection method of phenolic compound in a kind of carbonic ester packaging material for food according to claim 1 or 2, special
Sign is：1. step weighs 1mg target components in 10ml volumetric flasks, carry out constant volume with methanol, the standard for being made into 100mg/L is molten
Liquid is then stored in the environment of -20 DEG C.
4. the detection method of phenolic compound, feature in a kind of carbonic ester packaging material for food according to claim 1
It is：Step 5. in sample is cut by block using scissors first, then freezed using liquid nitrogen, then use freeze grinding
Instrument is ground it crushing.
5. the detection method of phenolic compound in a kind of carbonic ester packaging material for food according to claim 1 or 4, special
Sign is：Step 5. in weigh 2.0g after sample comminution and be placed in tool plug test tube, 10ml dichloromethane is added, ultrasonic extraction 1 is small
When, extracting solution is concentrated with Rotary Evaporators, after nitrogen drying, 1mL methanol dissolved residues is added, are carried out with 0.20 μm of miillpore filter
It is to be determined after filtering.
6. the detection method of phenolic compound, feature in a kind of carbonic ester packaging material for food according to claim 5
It is：Step 5. in step 5. in weigh 2.0g after sample comminution and be placed in tool plug test tube, 10ml dichloromethane is added, is taken the photograph 40
Ultrasonic extraction 1 hour under the conditions of family name's degree, extracting solution is concentrated with Rotary Evaporators, and after nitrogen drying, it is residual that the dissolving of 1mL methanol is added
Slag is filtered rear to be determined with 0.20 μm of miillpore filter.
7. the detection method of phenolic compound, feature in a kind of carbonic ester packaging material for food according to claim 1
Be, step 2. in liquid chromatogram mobile phase be A- methanol, B-0.1% ammonium hydroxide.
8. the detection method of phenolic compound in a kind of carbonic ester packaging material for food according to claim 1 or claim 7, special
Sign is that 2. middle gradient elution program is that 0 ~ 2min corresponds to the mobile phase of 80%A-20%B, 2 ~ 6min corresponds to 60%A-40%B to step
Mobile phase, 6 ~ 12min correspond to the mobile phase of 80%A-20%B.
9. the detection method of phenolic compound, feature in a kind of carbonic ester packaging material for food according to claim 1
It is：Step 3. in go the solvent gas and taper hole gas to be high pure nitrogen, flow velocity is respectively 500L/h and 50L/h.
10. the detection method of phenolic compound, feature in a kind of carbonic ester packaging material for food according to claim 1
It is：3. middle collision gas is high-purity argon gas to step.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109633070A (en) * | 2019-02-26 | 2019-04-16 | 江阴市产品质量监督检验所 | A kind of method that High Performance Liquid Chromatography detects nonyl phenol and bisphenol-A in Food Plastic Packaging Material |
| CN109738534A (en) * | 2019-01-10 | 2019-05-10 | 安徽省阜阳市国泰彩印包装有限公司 | A kind of color printing packing solvent method for detecting residue |
| CN110082437A (en) * | 2019-03-27 | 2019-08-02 | 中国检验检疫科学研究院 | The method for detecting bisphenol compound |
| CN111579670A (en) * | 2020-05-26 | 2020-08-25 | 亿科检测认证有限公司 | Method for detecting bisphenol F in food contact plastic product |
| CN116087374A (en) * | 2023-04-11 | 2023-05-09 | 农业农村部环境保护科研监测所 | Detection method for trace bisphenol compounds in agricultural products |
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| CN116087374A (en) * | 2023-04-11 | 2023-05-09 | 农业农村部环境保护科研监测所 | Detection method for trace bisphenol compounds in agricultural products |
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