CN105424855A - Method for measuring residual amount of anthraquinone in tea with gas chromatography-mass spectrum/mass spectrum method - Google Patents
Method for measuring residual amount of anthraquinone in tea with gas chromatography-mass spectrum/mass spectrum method Download PDFInfo
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Abstract
The invention relates to a method for measuring the residual amount of pollutants in tea, in particular to a method for measuring the residual amount of anthraquinone in tea with a gas chromatography-mass spectrum/mass spectrum method. The method for measuring the residual amount of anthraquinone in tea with the gas chromatography-mass spectrum/mass spectrum method includes the following steps of 1, sample processing; 2, measuring, wherein a standard working solution and a sample solution are injected under the set gas chromatography-mass spectrum/mass spectrum condition. The method for measuring the residual amount of anthraquinone in tea with the gas chromatography-mass spectrum/mass spectrum method is simple, convenient, rapid, accurate and reliable, and the limit of detection, the recovery rate and the precision degree all meet requirements.
Description
Technical field
The present invention relates to a kind of method measuring pollutant residual quantity in tealeaves, particularly relate to the method for anthraquinone residual quantity in a kind of gas chromatography-mass spectrum/mass spectroscopy tealeaves.
Background technology
Anthraquinone (AnthraquinoneAQ, CASNo84-65-1, C
14h
8o
2) be a kind of widely used chemical products.As the parent of dyes of anthraquinone, 9,10-anthraquinone is the parent of synthesis disperse dyes, acid dyes, reducing dye and reactive dye; As the adjuvant of paper-making process, 9,10-anthraquinone can accelerate the speed of delignification, improves paper pulp yield; Agriculturally, anthraquinone was once used as bird repellent and was applied to rice field and oil crops growing area, and current 9,10-anthraquinones all do not have registration for agricultural production again in European Union or other countries.In China, anthraquinone also registration use not on China tea tree and on other crops.Although AQ is considered to low toxicity, EFSA (EuropeanFoodSafetyAuthority) points out in reevaluating report, and AQ may exist carcinogenic risk.Its molecular structural formula is as follows:
European Union specifies that the maximum residue limit of anthraquinone in tealeaves (MRL) standard is 0.02mg/kg, and China does not specify the maximum residue limit of anthraquinone in tealeaves.Document has no report to anthraquinone in tealeaves.
Summary of the invention
In order to solve above-mentioned technical matters, the invention provides the method for anthraquinone residual quantity in a kind of gas chromatography-mass spectrum/mass spectroscopy tealeaves, the method is easy, stable, mensuration lower bound is 0.02mg/kg, and meet the requirement that domestic and international regulations is residual to anthraquinone in tealeaves completely, the supervision that can be tealeaves anthraquinone residual provides technical support.
In order to realize above-mentioned object, present invention employs following technical scheme:
The method of anthraquinone residual quantity in gas chromatography-mass spectrum/mass spectroscopy tealeaves, the method comprises the following steps:
1) sample preparation
Take tealeaves sample 2g, in 50mL centrifuge tube, add 0.5mL0.2 μ g/mL anthraquinone-D8 solution, add 20mL normal hexane-acetone soln again, normal hexane-acetone volume ratio is 1:1, with 10000r/min homogeneous 0.5min, add 2g sodium chloride, vortex 1min, with the centrifugal 3min of 4000r/min, upper strata being extracted solution is transferred in concentrated bottle, with 20mL normal hexane-acetone soln cleaning homogenizer cutter head, and this extract is poured in residue, vortex 1min, with the centrifugal 3min of 4000r/min, merge extract, below 45 DEG C, water-bath is evaporated near dry, with 3mL n-hexane dissolution residue, and be transferred to florisil silica decontaminating column, usually 50mL normal hexane-ether mixed solvent wash-out is used again, normal hexane-ether volume ratio 8:2, flow velocity is 3mL/min, collect whole eluent, below 45 DEG C, water-bath is evaporated near dry, add 2.0mL acetone solution residue, cross 0.22 μm of filter membrane, measure for gas chromatography-mass spectrum/mass spectrometer,
2) measure
Standard working solution and sample solution sample introduction under the gas chromatography-mass spectrum/Mass Spectrometry Conditions of following setting:
1. the mass spectrometry parameters of anthraquinone
Wherein * represents quota ion;
2. gas chromatography-mass spectrum/mass spectrographic instrument condition parameter
Gas chromatography:
Chromatographic column: HP-5MS, 30m length × 0.25mm internal diameter × 0.25 μm thickness
Program column temperature: 100 DEG C keep 1min, with the ramp to 300 DEG C of 20 DEG C/min, keeps 10min
Flow velocity: 1.0mL/min
Sample size: 1 μ L
Injection port temperature: 300 DEG C
Input mode Splitless injecting samples;
Mass Spectrometry Conditions:
Ionization mode: EI
Ionizing energy: 70eV
Ion source temperature: 280 DEG C
Level Four bar temperature: do not heat
Interface temperature: 300 DEG C
Mensuration mode: Selective reaction monitoring pattern (SRM);
The maximum allowable offset of relative abundance of ions during qualitative confirmation:
Relative ion abundance > 50%, relative deviation ± 20% of permission
Relative ion abundance > 20% ~ 50%, relative deviation ± 25% of permission
Relative ion abundance > 10% ~ 20%, relative deviation ± 30% of permission
Relative ion abundance≤10%, relative deviation ± 50% of permission;
3) blank test
Except not adding except sample, all by above-mentioned steps 1), step 2) operation steps carries out;
4) result calculates and statement
With chromatographic data processor or the content calculating anthraquinone in sample as follows, result of calculation must deduct blank value:
In formula:
X
i--the residual quantity of anthraquinone in sample, unit is milligrams per kilogram;
C
i--obtain the solution concentration of anthraquinone from typical curve, unit is micrograms per millilitre;
V--the final constant volume of sample liquid, unit is milliliter;
M--final sample mass representated by sample liquid, unit is gram;
5) judge
With mass concentration X for horizontal ordinate, peak area ratio Y is ordinate, draws 5 standard working curves, carries out quantitatively with standard working curve to sample, and the response of sample solution Chinese traditional medicine should in the range of linearity of instrument detection; Under above-mentioned chromatographic condition, corresponding measured object whether is there is in judgement sample, the following condition of demand fulfillment: the mass chromatography peak retention time occurred in sample solution is consistent with hybrid standard working fluid, permissible variation is less than ± and 0.5%, medicine corresponding to this chromatographic peak is consistent in the relative abundance of the relative abundance of the mass spectrometry ion mixed-matrix standard working solution suitable with concentration, relative abundance deviation is no more than above-mentioned regulation, then can determine containing this medicine.
As preferably, described florisil silica decontaminating column selects 200mm × 15mm internal diameter glass column, about 5mm height absorbent cotton and about 10mm height anhydrous sodium sulfate are padded in bottom, 10g florisil silica, the granularity of florisil silica 75 μm ~ 150 μm, 650 DEG C of calcination 4h, use 130 DEG C to activate 4h and be cooled to room temperature in exsiccators, add the water deactivation of 2%; Top adds about 10mm height anhydrous sodium sulfate, with normal hexane wet method dress post, discards leacheate.
Assay method of the present invention adopts anthraquinone residual quantity in gas chromatography-mass spectrum/mass spectrometric determination tealeaves, and method is easy, quick, accurate, reliable, and detectability, the recovery and precision all meet the requirements.
Assay method of the present invention has following technique effect:
1) develop the method for anthraquinone residual quantity in gas chromatography-mass spectrum/mass spectroscopy Simultaneously test tealeaves first, fill up technological gap;
2) optimal conditions of anthraquinone residual quantity in gas chromatography-mass spectrum/mass spectrometric determination cotton is provided.
Accompanying drawing explanation
Fig. 1 is the selectivity ion flow graph of anthraquinone and anthraquinone-D8 mixed standard solution.
Fig. 2 is the selectivity ion flow graph of blank Tea Samples and anthraquinone-D8 mixed solution.
Fig. 3 is the selectivity ion flow graph that blank Tea Samples adds anthraquinone and anthraquinone-D8 mixed standard solution (0.02mg/kg).
Embodiment
1, reagent and material
1.1 normal hexanes: chromatographically pure.
1.2 acetone: chromatographically pure.
1.3 ether: chromatographically pure.
1.4 sodium chloride: analyze pure, 650 DEG C of calcination 4h, are cooled to room temperature in exsiccator, store in air-tight bottle for subsequent use.
1.5 anhydrous sodium sulfates: analyze pure, 650 DEG C of calcination 4h, are cooled to room temperature in exsiccator, store in air-tight bottle for subsequent use.
1.6 anthraquinones, anthraquinone-D8 standard substance (Anthraquinone, CAS:84-65-1, C14H8O2; Anthraquinone-D8, CAS:10439-39-1): purity is more than or equal to 99%.
1.7 Standard Stock solutions: accurately take through appropriate standard substance (1.6), be mixed with the standard reserving solution of 0.4mg/mL with acetone, in 0 DEG C ~ 4 DEG C refrigerators, lucifuge stores, the term of validity 6 months.
1.8 anthraquinone-D8 Standard Stock solutions: accurately take through appropriate standard items (1.6), be mixed with the standard reserving solution of 0.4mg/mL with acetone, in 0 DEG C ~ 4 DEG C refrigerators, lucifuge stores, the term of validity 6 months.
The preparation of 1.9 standard intermediate liquids: accurately pipette standard reserving solution appropriate (1.7), be mixed with the standard solution of 10 μ g/mL with acetone; Accurately pipette standard reserving solution appropriate (1.8), the mixed standard solution lucifuge in 0 DEG C ~ 4 DEG C refrigerators being mixed with 0.2 μ g/mL with acetone stores, the term of validity 3 months.
The preparation of 1.10 standard working solution: the standard working solution as required standard intermediate solution (1.9) being become debita spissitudo by acetone diluted.
1.11 florisil silicas: granularity 75 μm ~ 150 μm (100 order ~ 200 order), 650 DEG C of calcination 4h, use 130 DEG C to activate 4h and be cooled to room temperature in exsiccators, add the water deactivation of 2%, for subsequent use.
1.12 decontaminating columns: 200mm × 15mm (internal diameter) glass column, about 5mm height absorbent cotton and about 10mm height anhydrous sodium sulfate are padded in bottom, 10g florisil silica (1.11), top adds about 10mm height anhydrous sodium sulfate, with normal hexane wet method dress post, discard leacheate (needing before use first to do elution curve).
1.13 miillpore filters: 0.22 μm, organic facies pattern.
2, instrument and equipment
2.1 gas chromatography-mass spectrums/mass spectrometer: be furnished with (EI) ion gun;
2.2 analytical balances: sensibility reciprocal 0.0001g and 0.01g;
2.3 turbine mixer;
2.4 homogenizer;
2.5 oscillator;
2.6 hydro-extractors: maximum (top) speed 4000r/min;
2.7 Rotary Evaporators;
2.8 comminutor.
3, determination step
3.1 sample pre-treatments
Take tealeaves sample 2g (being accurate to 0.01g) in 50mL centrifuge tube, add 0.5mL anthraquinone-D8 (0.2 μ g/mL), add 20mL normal hexane-acetone (1+1 again, volume ratio), with 10000r/min homogeneous 0.5min, add 2g sodium chloride, vortex 1min, with the centrifugal 3min of 4000r/min, upper strata being extracted solution is transferred in concentrated bottle, with 20mL normal hexane-acetone (1+1, volume ratio) clean homogenizer cutter head, and this extract is poured in residue, vortex 1min, with the centrifugal 3min of 4000r/min, merge extract, below 45 DEG C, water-bath is evaporated near dry, with 3mL n-hexane dissolution residue, and be transferred to florisil silica decontaminating column (1.12), usually 50mL normal hexane-ether (8+2 is used again, volume ratio) mixed solvent, flow velocity is 3mL/min, collect whole eluent, below 45 DEG C, water-bath is evaporated near dry, add 2.0mL acetone solution residue, cross 0.22 μm of filter membrane, measure for gas chromatography-mass spectrum/mass spectrometer.
3.2 measure
Because test condition depends on used instrument, the general parameter of stratographic analysis therefore can not be provided.It is suitable for adopting following operating conditions to be proved to be test.Design parameter is in table 2, table 3.
Table 2 gas chromatograph parameters
| Chromatographic column | HP-5MS, 30m (length) × 0.25mm (internal diameter) × 0.25 μm (thickness) |
| Program column temperature | 100 DEG C keep 1min, with the ramp to 300 DEG C of 20 DEG C/min, keep 10min |
| Flow velocity | 1.0mL/min |
| Sample size | 1μL |
| Injection port temperature | 300℃ |
| Input mode | Splitless injecting samples |
Table 3 Mass Spectrometry Conditions parameter
| Ionization mode | EI |
| Ionizing energy | 70eV |
| Ion source temperature | 280℃ |
| Level Four bar temperature | Do not heat |
| Interface temperature | 300℃ |
| Mensuration mode | Selective reaction monitoring pattern (SRM) |
4 blank tests
Except not adding except sample, all undertaken by aforesaid operations step.
5 results calculate and statement
With chromatographic data processor or the content pressing anthraquinone in formula (1) calculating sample, result of calculation must deduct blank value:
In formula:
X
i--the residual quantity of anthraquinone in sample, unit is milligrams per kilogram (mg/kg);
C
i--from the solution concentration of the anthraquinone that typical curve obtains, unit is micrograms per millilitre (μ g/mL);
V--the final constant volume of sample liquid, unit is milliliter (mL);
M--final sample mass representated by sample liquid, unit is gram (g);
6 measure lower bound
The mensuration lower bound of this method is 0.02mg/kg.
7 recovery
The experiment of this method recovery sets three and adds concentration, and by the determined experiment condition of this method, carry out 6 experiments to each interpolation concentration, the recovery and precision the results are shown in Table 4.
The interpolation concentration of table 4 sample and recovery scope
Claims (2)
1. in gas chromatography-mass spectrum/mass spectroscopy tealeaves, the method for anthraquinone residual quantity, is characterized in that the method comprises the following steps:
1) sample preparation
Take tealeaves sample 2g, in 50mL centrifuge tube, add 0.5mL0.2 μ g/mL anthraquinone-D8 solution, add 20mL normal hexane-acetone soln again, normal hexane-acetone volume ratio is 1:1, with 10000r/min homogeneous 0.5min, add 2g sodium chloride, vortex 1min, with the centrifugal 3min of 4000r/min, upper strata being extracted solution is transferred in concentrated bottle, with 20mL normal hexane-acetone soln cleaning homogenizer cutter head, and this extract is poured in residue, vortex 1min, with the centrifugal 3min of 4000r/min, merge extract, below 45 DEG C, water-bath is evaporated near dry, with 3mL n-hexane dissolution residue, and be transferred to florisil silica decontaminating column, usually 50mL normal hexane-ether mixed solvent wash-out is used again, normal hexane-ether volume ratio 8:2, flow velocity is 3mL/min, collect whole eluent, below 45 DEG C, water-bath is evaporated near dry, add 2.0mL acetone solution residue, cross 0.22 μm of filter membrane, measure for gas chromatography-mass spectrum/mass spectrometer,
2) measure
Standard working solution and sample solution sample introduction under the gas chromatography-mass spectrum/Mass Spectrometry Conditions of following setting:
1. the mass spectrometry parameters of anthraquinone
Wherein * represents quota ion;
2. gas chromatography-mass spectrum/mass spectrographic instrument condition parameter
Gas chromatography:
Chromatographic column: HP-5MS, 30m length × 0.25mm internal diameter × 0.25 μm thickness
Program column temperature: 100 DEG C keep 1min, with the ramp to 300 DEG C of 20 DEG C/min, keeps 10min
Flow velocity: 1.0mL/min
Sample size: 1 μ L
Injection port temperature: 300 DEG C
Input mode Splitless injecting samples;
Mass Spectrometry Conditions:
Ionization mode: EI
Ionizing energy: 70eV
Ion source temperature: 280 DEG C
Level Four bar temperature: do not heat
Interface temperature: 300 DEG C
Mensuration mode: Selective reaction monitoring pattern (SRM);
The maximum allowable offset of relative abundance of ions during qualitative confirmation:
Relative ion abundance > 50%, relative deviation ± 20% of permission
Relative ion abundance > 20% ~ 50%, relative deviation ± 25% of permission
Relative ion abundance > 10% ~ 20%, relative deviation ± 30% of permission
Relative ion abundance≤10%, relative deviation ± 50% of permission;
3) blank test
Except not adding except sample, all by above-mentioned steps 1), step 2) operation steps carries out;
4) result calculates and statement
With chromatographic data processor or the content calculating anthraquinone in sample as follows, result of calculation must deduct blank value:
In formula:
X
i--the residual quantity of anthraquinone in sample, unit is milligrams per kilogram;
C
i--obtain the solution concentration of anthraquinone from typical curve, unit is micrograms per millilitre;
V--the final constant volume of sample liquid, unit is milliliter;
M--final sample mass representated by sample liquid, unit is gram;
5) judge
With mass concentration X for horizontal ordinate, peak area ratio Y is ordinate, draws 5 standard working curves, carries out quantitatively with standard working curve to sample, and the response of sample solution Chinese traditional medicine should in the range of linearity of instrument detection; Under above-mentioned chromatographic condition, corresponding measured object whether is there is in judgement sample, the following condition of demand fulfillment: the mass chromatography peak retention time occurred in sample solution is consistent with hybrid standard working fluid, permissible variation is less than ± and 0.5%, medicine corresponding to this chromatographic peak is consistent in the relative abundance of the relative abundance of the mass spectrometry ion mixed-matrix standard working solution suitable with concentration, relative abundance deviation is no more than above-mentioned regulation, then can determine containing this medicine.
2. the method for anthraquinone residual quantity in gas chromatography-mass spectrum according to claim 1/mass spectroscopy tealeaves, it is characterized in that: florisil silica decontaminating column selects 200mm × 15mm internal diameter glass column, about 5mm height absorbent cotton and about 10mm height anhydrous sodium sulfate are padded in bottom, 10g florisil silica, the granularity of florisil silica 75 μm ~ 150 μm, 650 DEG C of calcination 4h, use 130 DEG C to activate 4h and be cooled to room temperature in exsiccators, add the water deactivation of 2%; Top adds about 10mm height anhydrous sodium sulfate, with normal hexane wet method dress post, discards leacheate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106841481A (en) * | 2017-03-28 | 2017-06-13 | 中国农业科学院茶叶研究所 | The method that solid phase dispersion purification techniques quickly determines 9,10 anthraquinone residual quantities in tealeaves |
| CN108414652A (en) * | 2018-02-09 | 2018-08-17 | 中国农业科学院茶叶研究所 | The detection method of anthracene and its oxide anthraquinone, anthrone content in multi-interfacial feature |
| CN108680669A (en) * | 2018-05-08 | 2018-10-19 | 江苏安舜技术服务有限公司 | The test method of anthraquinone in a kind of plant-derived product and food |
| CN115261170A (en) * | 2022-09-05 | 2022-11-01 | 惠风酒业发展(上海)有限公司 | Distiller's yeast and health rice wine |
| CN117420256A (en) * | 2023-10-16 | 2024-01-19 | 上海国齐检测技术有限公司 | Method for detecting anthraquinone compounds and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106841481A (en) * | 2017-03-28 | 2017-06-13 | 中国农业科学院茶叶研究所 | The method that solid phase dispersion purification techniques quickly determines 9,10 anthraquinone residual quantities in tealeaves |
| CN108414652A (en) * | 2018-02-09 | 2018-08-17 | 中国农业科学院茶叶研究所 | The detection method of anthracene and its oxide anthraquinone, anthrone content in multi-interfacial feature |
| CN108414652B (en) * | 2018-02-09 | 2021-06-25 | 中国农业科学院茶叶研究所 | Method for detecting content of anthracene and anthraquinone and anthrone oxides thereof in multi-medium environment |
| CN108680669A (en) * | 2018-05-08 | 2018-10-19 | 江苏安舜技术服务有限公司 | The test method of anthraquinone in a kind of plant-derived product and food |
| CN115261170A (en) * | 2022-09-05 | 2022-11-01 | 惠风酒业发展(上海)有限公司 | Distiller's yeast and health rice wine |
| CN117420256A (en) * | 2023-10-16 | 2024-01-19 | 上海国齐检测技术有限公司 | Method for detecting anthraquinone compounds and application thereof |
| CN117420256B (en) * | 2023-10-16 | 2024-06-04 | 上海国齐检测技术有限公司 | Method for detecting anthraquinone compounds and application thereof |
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