CN103499668B - UPC<2> (ultra performance convergence chromatographic) analysis method for detecting DEAB and MK in printing and packaging material - Google Patents
UPC<2> (ultra performance convergence chromatographic) analysis method for detecting DEAB and MK in printing and packaging material Download PDFInfo
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Abstract
The invention discloses a UPC<2> (ultra performance convergence chromatographic) analysis method for detecting DEAB and MK in a printing and packaging material. The method is characterized by comprising the following steps of extracting remaining DEAB and remaining MK in a sample substrate by using acetonitrile, performing separation by using UPC<2> after extraction liquid is filtered by an organic phase filter membrane, and performing detection by using an ultraviolet detector to finally determine the DEAB content and the MK content of a printing and packaging material sample. The method has the effects that a UPC<2> technology is used for the first time, an analysis method for the DEAB and the MK in the printing and packaging material is established, two similar compounds can be effectively separated and quantified within 4 minutes by the analysis method, and compared with a conventional common analysis method, the analysis method has the advantage that the detection time is remarkably shortened; carbon dioxide is adopted as a main flowing phase, and the consumption of an organic solvent is extremely low, so that the requirements of environment-friendly analysis and detection are better met; a gas flowing phase with lower cost is adopted, and meanwhile, the analysis time is short, so that the detection and analysis cost is greatly lowered; the method is high in sensitivity, accuracy and repeatability.
Description
Technical field
The invention belongs to physical and chemical inspection technical field, the ultra high efficiency relating to 4,4-two (diethylamino) benzophenone (DEAB) and two (dimethylamino) benzophenone (MK) of 4,4-in printed apcksging material specifically closes analysis of hplc method.
Background technology
4, two (diethylamino) benzophenone (DEAB) and 4 of 4-, two (dimethylamino) benzophenone (MK) of 4-is important ultraviolet (UV) absorbing agent and initiating agent, and widely use in UV ink, be also one of important pollutant index of deinking recycled fiber recycled writing paper simultaneously.2007, European Union was at the few members state Res AP(2002 of " about intending and the paper and paperboard material of Food Contact and goods ") resolve in 1, clearly forbid using DEAB and MK in the printing-ink of food contact material
[1].
Ultra high efficiency closes phase chromatogram (Ultra performance convergence chromatography, UPC
2)
[2]technology is a kind of isolation technics proposed recently, and it comes from supercritical fluid chromatography technology, because it is with supercritical carbon dioxide (CO
2) be main mobile phase, therefore have that viscosity is low, mass-transfer performance good, separation efficiency is high, the advantage of environmental protection; Meanwhile, this system is based on the UPLC of Waters maturation
tMtechnology platform, and the chromatographic column chemical technology of sub-2 μm, what make instrument can have the progress of a matter in the aspect such as handling, reappearance, precision.
At present, the domestic analytical approach bibliographical information that yet there are no these two kinds of compounds, the common method about light trigger analysis has GC-MS(gas chromatography-mass spectrography), liquid phase chromatography and ultra-performance liquid chromatography
[3 ~ 7].But it is longer all to there is sample analysis time in correlation analysis method, the shortcoming that analytic process is loaded down with trivial details.In addition, adopt during liquid chromatography analysis and need to consume a large amount of organic solvent, do not meet the development trend of environmental protection analytical approach.Applicant in this case applied for " measuring the detection method of 16 kinds of light triggers in paper printed matter " in August, 2012, the method take gas chromatography-mass spectrum as analytical instrument, in 40 minutes, effectively can analyze 16 kinds of light triggers in paper printed matter, wherein also include DEAB and MK two kinds of materials.Above-mentioned is that the method for analytical instrument will with expensive high-purity helium for mobile phase with gas chromatography-mass spectrum, and inspection cost is high.A kind of easy, quick, accurate, lower-cost detection method can be provided, cause the concern of various equivalent modifications.
summary of the invention:
Object of the present invention is intended to overcome prior art defect, and adopt acetonitrile to extract DEAB and MK residual in sample substrate, extract, after organic phase membrane filtration, utilizes UPC
2be separated, UV-detector detects.The present invention finally provides the analytical approach of DEAB and MK in a kind of easy, quick, Accurate Determining printed apcksging material, in associated materials, the fast quantitative measurement method for detecting of DEAB and MK provides foundation.
The object of the invention is to be realized by following concrete steps:
The ultra high efficiency detecting DEAB and MK in printed apcksging material closes an analysis of hplc method, and concrete steps are as follows:
(1) sample preparation
Accurately cut 0.5 dm
2paper printing packaging sample, and be cut into the fragment of 0.5 cm × 0.5 cm, be placed in 50 mL tool plug triangular flasks, as paper printing packaging sample specimens.
(2) extraction of sample
The Extraction solvent adopted is acetonitrile or acetonitrile solution, and wherein in acetonitrile solution, the ratio of acetonitrile is not less than 50%, and Extraction solvent addition is 20 ~ 50 mL.Adopt after effective means extracts sample, by extract with after 0.22 μm of membrane filtration, obtain filtrate and can carry out UPC
2analyze.
When adopting ultrasonic extracting mode, ultrasonic power is at 40 ~ 100 Hz, and extraction time is 30 ~ 50 minutes; When adopting mechanical shaking extraction mode, extraction time is 1 ~ 2 h; When adopting accelerated solvent extractor mode, extraction time is 10 minutes, and temperature is 40 DEG C, and pressure is 1500 psi; When adopting immersion to leave standstill extraction, soak time is no less than 12 h.
(3) preparation of standard working solution
The preparation of standard working solution is divided into three steps, first prepares the standard items stock solution of each material; Secondly get single standard product stock solution constant volume in volumetric flask of certain volume respectively, obtain the mixed standard solution of DEAB and MK; Last actual content per sample needs, and stepwise dilution mixed standard solution obtains series standard working solution.
The compound method of single standard product stock solution in this step: accurately take 50 mg DEAB and MK respectively to the different brown volumetric flasks of 10 mL, be accurate to 0.1 mg, dissolve with acetonitrile and distinguish constant volume, be mixed with the single standard product storing solution that concentration is 5 mg/mL, at-18 DEG C of condition lower seal stored protected from light.The term of validity 6 months.
The compound method of mixed standard solution in this step: accurately pipette 1 mL mono-standard items stock solution respectively in the brown volumetric flask of 50 mL, scale is settled to acetonitrile, being mixed with concentration is 100 mg/L mixed standard solutions, at-18 DEG C of condition lower seal stored protected from light.
The recommendation compound method of series standard working solution in this step: need the series standard working solution preparing suitable concn per sample.Series standard working solution should take acetonitrile as solvent, adopts mixed standard solution dilution to prepare series standard working solution.Recommend following compound method: accurately pipette 0.05 mL, 0.1 mL, 0.2 mL, 0.4 mL, 1 mL, 2 mL mixed standard solutions respectively in 6 brown volumetric flasks of 10 mL, use acetonitrile constant volume, obtain series standard working solution, the series standard solution concentration of preparation is 0.5 mg/L, 1 mg/L, 2 mg/L, 4 mg/L, 10 mg/L, 20 mg/L.
(4) instrumental analysis: adopt conjunction phase chromatogram to be separated, UV-detector detects, quantified by external standard method.
Chromatographic condition: chromatographic column can select ACQUITY UPC
2bEH chromatographic column (1.7 μm, 3 mm × 100 mm), ACQUITY UPC
2bEH 2-EP chromatographic column (1.7 μm, 3 mm × 150 mm), ACQUITY UPC
2hSS C18 SB chromatographic column (1.8 μm, 3 mm × 150 mm) and ACQUITY UPC
2arbitrary money in CSH Fluoro-Phenyl Column chromatographic column (1.7 μm, 3 mm × 150 mm); ABPR pressure is 1600 ~ 1800 psi; Chromatogram column temperature is 40 ~ 60 DEG C; Sample size is 2 ~ 5 μ L; Mobile phase is respectively carbon dioxide (mobile phase A) and methyl alcohol (Mobile phase B), and flow velocity is 1.5 mL/min, and eluent gradient is as table 1, and UV detect wavelength is 348 nm.According to above-mentioned condition, under the mixed standard solution 348 nm testing conditions obtained, chromatogram is as Fig. 2.
table 1 gradient elution program
(5) result calculates
In paper printing material sample, the content of DEAB and MK calculates by formula (1):
………………………（1）
In formula:
c i ---the content of DEAB or MK in sample, unit is milligram every square metre (mg/m
2);
c---the concentration of DEAB or MK in sample solution, unit is milligrams per liter (mg/L);
c 0 ---the concentration of DEAB or MK in blank sample, unit is milligrams per liter (mg/L);
v
---the extract volume that extraction sample is used, unit is milliliter (mL);
s---the area of sample, unit is square decimeter (dm
2).
Compared with prior art, instant invention overcomes the deficiency of prior art sample treatment, optimize instrument testing conditions, the present invention has following effect:
(1) the present invention utilizes UPC first
2technology, establishes the analytical approach of DEAB and MK in printed apcksging material.
(2) analytical approach of the present invention can realize effective separation of 2 kinds of analogue compounds with quantitative in 4 minutes, and compare analytical approach conventional at present, detection time significantly shortens.
(3) the main mobile phase that analytical approach of the present invention adopts is carbon dioxide, and organic solvent consumption is few, thus more meets the requirement that detection is analyzed in environmental protection.
(4) analytical approach of the present invention is owing to have employed more cheap gas mobile phase, and analysis time is very short simultaneously, detects analysis cost therefore, it is possible to greatly reduce.
(5) sensitivity of analytical method of the present invention and accuracy high, reproducible.
Compared with the patent of applying in August, 2012 with the applicant, the present invention is directed to DEAB and MK comparatively paid close attention at present, utilize UPC first
2technology establishes the analytical approach of DEAB and MK in a kind of printed apcksging material.This technology is with carbon dioxide (CO
2) be main mobile phase, separation and the quantitative test of two kinds of compounds can be realized in 3 ~ 4 minutes, analysis time, declaration method shortened nearly 10 times more, greatly reduce inspection cost simultaneously, meet the requirement of environmental protection inspection, foundation can be provided for the quick and precisely check analysis of this index.
Accompanying drawing explanation
Fig. 1 assay method process flow diagram of the present invention.
Fig. 2 is different, and chromatographic column is separated exemplary plot.
Note: 1:DEAB, 2:MK.A:ACQUITY UPC
2bEH chromatographic column (1.7 μm, 3 mm × 100 mm); B:ACQUITY UPC
2bEH 2-EP chromatographic column (1.7 μm, 3 mm × 150 mm); C:ACQUITY UPC
2hSS C18 SB chromatographic column (1.8 μm, 3 mm × 150 mm); D:ACQUITY UPC
2cSH Fluoro-Phenyl Column chromatographic column (1.7 μm, 3 mm × 150 mm).
Fig. 3 chromatogram column temperature selects exemplary plot.
Fig. 4 ABPR pressure selection exemplary plot.
Fig. 5 is separated solvent and selects exemplary plot.
Fig. 6 standard solution chromatogram exemplary plot.
In Fig. 3-6: 1:DEAB, 2:MK.
Embodiment
The present invention is described further in conjunction with example, but is not restriction the present invention.
Example 1:
1) chromatographic condition
Chromatographic column is adopted to be Acquity UPC
2cSH Fluoro-Phenyl chromatographic column; System back pressure is 1800 psi; Chromatogram column temperature is 50 DEG C; Sample size is 3 μ L; Mobile phase is respectively carbon dioxide (mobile phase A) and methyl alcohol (Mobile phase B); Column flow rate is 1.5 mL/min; Eluent gradient elution program is as table 1 listed hereinbefore.Ultraviolet wavelength 348 nm is adopted to monitor.
2) preparation of standard solution
Accurately take the various light trigger of 50 mg respectively, be accurate to 0.1 mg, dissolve with acetonitrile and distinguish constant volume in the brown volumetric flask of 10 mL, being prepared into the single standard product storing solution that concentration is 5 mg/mL.Then accurately pipette 1 mL single standard product stock solution respectively in the brown volumetric flask of 50 mL, be settled to scale with acetonitrile, being prepared into concentration is 100 mg/L mixed standard solutions.Take acetonitrile as solvent, adopt the standard solution of mixed standard solution dilution method preparation 0.5,1,2,5,10 mg/L, set up equation of linear regression with the corresponding standard working solution concentration of standard series peak area.
3) sample preparation
Accurately cut 0.5 dm
2packaging sample, be cut into the fragment being not more than 0.5 cm × 0.5 cm, be placed in 50 mL tool plug triangular flasks, accurately add 20 mL acetonitrile solutions, ultrasonic extraction 40 min, extract directly carries out UPC after organic membrane filter
2systematic analysis.According to above-mentioned condition, under the mixed standard solution 348 nm testing conditions obtained, chromatogram is as Fig. 2.
4) actual sample analysis
Adopt this method to detect the paper wrapper that 5 kinds adopt UV typography to produce, testing result (as table 2) shows, detected DEAB, but content is relatively low in 2 samples.
table 2 actual sample testing result (unit: mg/m
2
)
| Sample | DEAB | MK |
| Wine packing box 1 | 1.65 | — |
| Wine packing box 2 | — | — |
| Box for moon-cake | — | — |
| Tobacco shred wrapping paper 1 | 1.06 | — |
| Tobacco shred wrapping paper 2 | — | — |
Note: "-" representative does not detect
With the better concrete scheme defined in the preferred the present invention of each examples comparative mode below the present invention:
Example 2:
UPC
2the kind of system chromatographic column used is many, contains the chromatographic column classification of positive and reversed-phase liquid chromatography (LC), and therefore, first the present invention investigates different chromatographic column to the impact be separated.This experimental selection 4 sections of obvious chromatographic columns of difference carry out conditional filtering, are respectively ACQUITY UPC
2bEH, ACQUITY UPC
2bEH 2-EP, ACQUITY UPC
2hSS C18 SB and ACQUITY UPC
2cSH Fluoro-Phenyl.From experimental result (Fig. 2), 4 sections of chromatographic columns can both reach good separating effect for these two kinds of materials, and 4 sections of chromatographic columns to the reserve capability of DEAB and MK are: CSH Fluoro-Phenyl>HSS C18 SB> BEH 2-EP > BEH.With this, the chromatographic column required by last right of the present invention can be a in 4 sections of chromatographic columns.
Example 3:
The present invention has investigated different pressures (1600 psi, 1800 psi and 2000 psi) and different chromatogram column temperature (40 DEG C, 50 DEG C and the 60 DEG C) impact on separating effect.Experimental result shows (as Fig. 3 ~ 4), and under the temperature and pressure of experiment, two kinds of compounds can be well separated.But too high pressure can cause the pressure closing phase chromatographic system to raise, thus exceeds the requirement of withstand voltage of instrument itself.Be 40 ~ 60 DEG C with the chromatogram column temperature used required by this last right of the present invention, post pressure is 1600-1800psi.
Example 4:
UPC
2mobile phase that system uses is mainly CO
2, and be separated using a small amount of organic solvent as cosolvent; The classification of its organic solvent is extensive, can contain the solvent kind of positive and negative phase LC, provide different selectivity and eluting power, and produces material impact to the separation of object.Experiment has been investigated 4 kinds of different organic solvents (methyl alcohol, ethanol, acetonitrile and isopropyl alcohol) and has been separated impact to 2 kinds of compounds.As seen from Figure 5,4 kinds of solvents to the eluting power of DEABG and MK are in the method: methyl alcohol > ethanol > acetonitrile > isopropyl alcohol.In addition, experiment also finds, ethanol, acetonitrile and isopropanol solvent are large due to viscosity, easily cause the back-pressure of system excessive, simultaneously the peak shape broadening that obtains of acetonitrile and isopropanol solvent auxiliary agent have conditions of streaking, and peak shape is relatively poor.Therefore, the final methyl alcohol that adopts of experiment is as organic solvent auxiliary flow phase.
Example 5
Adopt 3D detecting pattern, carry out the scanning of ultraviolet all band to single standard items of 2 kinds of materials, scanning wavelength scope is 210 ~ 400 nm.The uv-absorption maximum wavelength obtaining DEAB and MK is 353 and 343 nm.In order to take into account detection efficiency and method sensitivity, experiment employing 348 nm is determined wavelength, as shown in Figure 6.
Example 6
According to the preparation standard working solution method that the inventive method is recommended, and according to the instrument condition of the inventive method, sample size is 3 μ L, and UV detect wavelength is 348 nm, and the standard solution of series is carried out UPC
2after analysis, with external standard method drawing standard curve, ordinate is the peak area of each compound, and horizontal ordinate is the concentration (mg/L) of each compound, makes the standard working curve of two kinds of materials.The retention time of DEAB and MK, equation of linear regression, the range of linearity, related coefficient, method detection limit (stepwise dilution sample mark-on solution calculates according to signal to noise ratio (S/N ratio) S/N=3 and obtains) are in table 3.
As can be seen from the result of method evaluation, each compound separation is good, and this method sensitivity is higher, the good (R of place 0.5 ~ 20 mg/L concentration level scope internal linear relation
2>0.998), the detection demand of 2 kinds of restricted substances residual quantities in associated materials is met.
Example 7:
To the known printed wrapper sample not containing object, (paperboard material sample is quantitatively 275 g/m
2) carry out high, medium and low variable concentrations level standard solution recovery of standard addition test.The sample-pretreating method adopted is for accurately to cut 0.5 dm
2packaging sample, be cut into the fragment being not more than 0.5 cm × 0.5 cm, be placed in 50 mL tool plug triangular flasks, accurately add 20 mL acetonitrile solutions, ultrasonic extraction 40 min, extract directly carries out UPC after organic membrane filter
2systematic analysis.Each sample determination 5 times, the recovery and withinday precision measurement result are in table 4.As can be seen from the evaluation result of method, this method average recovery rate is 84.3 ~ 97.7%, and repeatability (RSD) is less than 6.1%, illustrates that this method can meet methodological evaluation requirement.
Example 8
The inventive method is utilized to detect 20 kinds of paper, cardboard, carton and paper-plastic stick printing packaging sample, experimental result and applicant in this case apply in August, 2012 compared with " measuring the detection method of 16 kinds of light triggers in paper printed matter " result, have good reproducibility; Meanwhile, because the inventive method have employed current comparatively advanced UPC
2technology, overcomes the shortcoming of conventional gas phase chromatogram and LC, can effective separation of realize target thing within very short analysis time; Have employed CO simultaneously
2as main mobile phase, therefore the advantage of environmental protection and energy consumption aspect is given prominence to.Can predict, the technology of the present invention has extremely wide prospect in the application and expansion in following correlation analysis field.
list of references
[1] Policy statement concerning paper and board materials and articles intended to come into contact with foodstuffs of 02 December 2009. http://www.foodcontactmaterials.com/materials/policy%20document%20paper.pdf, 02 December
2009
[2] Xu Yongwei, Sun Qinglong, Huang Jing, Tan Xiaojie, modern instrument, 2012,18 (5): 45-48.
[3] Morlock G., Schwack W., Anal. Bioanal. Chem., 2006, 385(3): 586-595.
[4] Benetti C., Angeletti R., Binato G., Biancardi A., Biancotto G., Anal. Chim. Acta, 2008, 617(1): 132-138.
[5] Sanches-Silva A., Pastorelli S., Cruz J, Simoneau C., Castanheira I., Paseiro-Losada P., J.Dairy. Sci., 2008, 91(3): 900-909.
[6] Zhang Yaohai, Jiao Bining, Zhou Zhiqin, analytical chemistry, 2012,40 (10): 1536-1542.
[7] Li Zhonghao, Tang Gangling, Wang Qinghua etc., modern food science and technology. 2011,27 (10): 1276-1280.
Claims (4)
1. the ultra high efficiency detecting DEAB and MK in printed apcksging material closes an analysis of hplc method, it is characterized in that: adopt acetonitrile to extract DEAB and MK residual in sample substrate, extract, after organic phase membrane filtration, utilizes UPC
2be separated, UV-detector detects, and finally determine the content of DEAB and MK in printed apcksging material sample, concrete steps are as follows:
(1) sample preparation
Accurately cut 0.5 dm
2paper printing packaging sample, and be cut into the fragment of 0.5 cm × 0.5 cm, be placed in 50 mL tool plug triangular flasks, as paper printing packaging sample specimens;
(2) extraction of sample
Adopt Extraction solvent acetonitrile or acetonitrile solution, in acetonitrile solution, the ratio of acetonitrile is not less than 50%, and Extraction solvent addition is 20 ~ 50 mL, extracts sample specimens, by extract with after 0.22 μm of membrane filtration, obtain filtrate and namely carry out UPC
2analyze;
(3) preparation of standard working solution
Preparation has the standard working solution of gradient concentration series, and the series standard solution concentration of preparation is 0.5 mg/L, 1 mg/L, 2 mg/L, 4 mg/L, 10 mg/L, 20 mg/L;
(4) instrumental analysis: adopt conjunction phase chromatogram to be separated, UV-detector detects, quantified by external standard method;
Chromatographic condition: chromatographic column selects ACQUITY UPC
2bEH chromatographic column specification 1.7 μm, 3 mm × 100 mm, ACQUITY UPC
2bEH 2-EP chromatographic column specification 1.7 μm, 3 mm × 150 mm, ACQUITY UPC
2hSS C18 SB chromatographic column specification 1.8 μm, 3 mm × 150 mm and ACQUITY UPC
2cSH Fluoro-Phenyl Column chromatographic column specification 1.7 μm, the arbitrary money in 3 mm × 150 mm; ABPR pressure is 1600 ~ 1800 psi; Chromatogram column temperature is 40 ~ 60 DEG C; Sample size is 2 ~ 5 μ L; Mobile phase is respectively A: carbon dioxide and B: methyl alcohol, and flow velocity is 1.5 mL/min, and eluent gradient elution program is: initial: 100%A, 0%B, curve: initial; 2 min:90%A, 10%B, curve: 6; 4 min:70%A, 30%B, curve: 6; 5 min:70%A, 30%B, curve: 6; 6 min:100%A, 0%B, curve: 6; UV detect wavelength is 348 nm;
Result calculates
In paper printing material sample, the content of DEAB and MK calculates by formula (1):
………………………（1）
In formula:
c i ---the content of DEAB or MK in sample, unit is milligram every square metre (mg/m
2);
c---the concentration of DEAB or MK in sample solution, unit is milligrams per liter (mg/L);
c 0 ---the concentration of DEAB or MK in blank sample, unit is milligrams per liter (mg/L);
v
---the extract volume that extraction sample is used, unit is milliliter (mL);
s---the area of sample, unit is square decimeter (dm
2).
2. in detection printed apcksging material according to claim 1, the ultra high efficiency of DEAB and MK closes analysis of hplc method, it is characterized in that: when adopting ultrasonic extracting mode, ultrasonic power is at 40 ~ 100 Hz, and extraction time is 30 ~ 50 minutes; When adopting mechanical shaking extraction mode, extraction time is 1 ~ 2 h; When adopting accelerated solvent extractor mode, extraction time is 10 minutes, and temperature is 40 DEG C, and pressure is 1500 psi; When adopting immersion to leave standstill extraction, soak time is no less than 12 h.
3. in detection printed apcksging material according to claim 1, the ultra high efficiency of DEAB and MK closes analysis of hplc method, it is characterized in that: the preparation of standard working solution is divided into three steps, first prepares the standard items stock solution of each material; Secondly get single standard product stock solution constant volume in volumetric flask of certain volume respectively, obtain the mixed standard solution of DEAB and MK; Last actual content per sample needs, and stepwise dilution mixed standard solution obtains series standard working solution.
4. in detection printed apcksging material according to claim 3, the ultra high efficiency of DEAB and MK closes analysis of hplc method, it is characterized in that: the compound method of single standard product stock solution: accurately take 50 mg DEAB and MK respectively to the different brown volumetric flasks of 10 mL, be accurate to 0.1 mg, dissolve with acetonitrile and distinguish constant volume, be mixed with the single standard product storing solution that concentration is 5 mg/mL, at-18 DEG C of condition lower seal stored protected from light, the term of validity 6 months, the compound method of mixed standard solution: accurately pipette 1 mL single standard product stock solution respectively in the brown volumetric flask of 50 mL, be settled to scale with acetonitrile, being mixed with concentration is 100 mg/L mixed standard solutions, at-18 DEG C of condition lower seal stored protected from light, the compound method of series standard working solution: need the series standard working solution preparing suitable concn per sample, series standard working solution take acetonitrile as solvent, mixed standard solution dilution is adopted to prepare series standard working solution, compound method: accurately pipette 0.05 mL respectively, 0.1 mL, 0.2 mL, 0.4 mL, 1 mL, 2 mL mixed standard solutions are in 6 brown volumetric flasks of 10 mL, use acetonitrile constant volume, obtain series standard working solution, the series standard solution concentration of preparation is 0.5 mg/L, 1 mg/L, 2 mg/L, 4 mg/L, 10 mg/L, 20 mg/L.
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| CN106896175B (en) * | 2017-03-10 | 2019-04-12 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of Ling " for giving up smoking |
| CN106814155B (en) * | 2017-03-10 | 2019-05-17 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of tomato |
| CN106841454B (en) * | 2017-03-10 | 2019-05-10 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of bolete |
| CN106896174B (en) * | 2017-03-10 | 2019-04-12 | 国家烟草质量监督检验中心 | The chiral analysis of nicotine closes phase chromatographic tandem mass spectrography in a kind of smoke-free tobacco product |
| CN107894487B (en) * | 2017-12-29 | 2020-03-27 | 国家烟草质量监督检验中心 | Method for detecting photoinitiator in printing 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 |
| CN115266999A (en) * | 2022-08-05 | 2022-11-01 | 陇南市祥宇油橄榄开发有限责任公司 | Qualitative and quantitative detection method for gamma-oryzanol in vegetable oil |
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