CN103323548A - Measurement method for residual amount of pentachlorophenol in cigarette paper - Google Patents
Measurement method for residual amount of pentachlorophenol in cigarette paper Download PDFInfo
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Abstract
A measurement method for the residual amount of pentachlorophenol in cigarette paper is characterized by comprising the following steps: cutting cigarette paper into pieces, adding extract liquor into the pieces, conducting ultrasonic extraction and measuring the residual amount of pentachlorophenol in the cigarette paper with liquid chromatography-tandem mass spectrometry (LC-MS/MS) directly after centrifugation of the extract liquor. The method comprises the following steps: a. cutting a cigarette paper sample according to relevant regulations; b. extracting a sample; c. purifying the sample; d. preparing a standard operating solution; e. carrying out liquid chromatography-tandem mass spectrometry (LC-MS/MS) measurement; f. calculating the measured result of the residual amount of pentachlorophenol. In comparison with the prior art, the measurement method has the following advantages: 1. adopting a pre-treatment of cutting the sample to make a solvent contact the sample better. The experiment result shows that such treatment can help to increase the extraction efficiency of pentachlorophenol. 2. measuring the content of pentachlorophenol in the paper with LC-MS/MS without derivatization operation, and the pre-treatment method is simple. 3. The method is accurate in operations, high in sensitivity and good in repeatability.
Description
Technical field
The invention belongs to the residual physical and chemical inspection technical field of objectionable impurities in the cigarette paper using, relate generally to the assay method of In Determination of Residual Pentachlorophenol in tobacco lining paper, tipping paper, the bar box packaging paper, a kind of employing ultrasonic extraction pentachlorophenol specifically, with the direct method for measuring of liquid chromatography-tandem mass spectrometry.
Background technology
Paper bag is drawn together in the production run of internal lining paper, tipping paper, bar box packaging paper etc., needs to add the chemicals such as various chemicals such as bleaching agent, processing aid, printing-ink, anticorrosion and bactericidal agent, to improve its packaging character and aesthetic property.But the research discovery, these chemicals can remain in the paper, and then move in the cigarette, and some of them migration thing has toxicity even carcinogenesis, to consumer's health formation harm.The developed countries such as the U.S., European Union, Japan have been all to having formulated corresponding rules and limit standard with the wrappage of Food Contact, and have implemented strict market access management.Pentachlorophenol (PCP) is used as the anticorrosion and mildewproof agent of wood raw material, can stop the growth of fungi, bacterium, suppresses corrosion.But pentachlorophenol has stronger toxicity, suck or absorb pentachlorophenol through skin and can cause headache, tired, the irritation of eyes, mucous membrane and skin, neuralgia, hidrosis, expiratory dyspnea, liver, renal damage etc. can produce biological accumulation in human body, Gamma Magnitude just can cause human body reproduction and development toxicity.Environmental Protection Agency and European Union have classified PCP as one of persistence organic pollutant of preferential control.Although PCP still may be present in other local imported raw material, be under an embargo in the product in European Union's scope at present.
Pentachlorophenol (pentachlorophenol, PCP) is a kind of common easily ionizable, be insoluble in the chlorinated aromatic organic contaminant of water.The pentachlorophenol stable chemical nature, under the usual conditions, pentachlorophenol is not oxidized, also is difficult to hydrolysis.Pentachlorophenol is dissociable in neutral and alkaline solution becomes the ionic state form, and in acid solution, it is still take molecular state as main.
At present to the mensuration of pentachlorophenol mainly in fields such as water, textile, soil, toy and articles for children, food plastic wrappage and medical supplies.Owing to containing hydroxyl on the phenyl ring in the chlorinated phenol chemical constitution, the polarity of molecule is strengthened, boiling point needs just can carry out gas chromatography or GC-MS(gas chromatography-mass spectrography) analysis [mensuration the 1st ~ 2 part of GB/T 18414.1-2-2006 textile chlorinated phenol: vapor-phase chromatography behind the derivatization up to 315 ℃; The mensuration gas chromatography-mass spectrography of pentachlorophenol in SN/T 2276-2009 food contact material paper pulp, paper and the cardboard aqueous extract; The mensuration of pentachlorophenol in GB/T 25002-2010 paper, cardboard and the pulp-water extract; ISO 15320:2011].The derivatization process is complicated, and expends that reagent is many and toxicity is large.High performance liquid chromatography has that separation efficiency is high, and analysis speed is fast, operates simple and easyly, is particularly suitable for the analysis of higher boiling, poor heat stability, strong polar material.The LC-MS/MS method [phenolic compound in the Ultra Performance Liquid Chromatography one series connection mass spectrometric determination food wrapper, the analytical test journal, 2012,29(12), 1153; The flood Aiwa, Yin Pinghe.Tablets by HPLC-MS is measured the chlorinated phenol in the textile, the assay laboratory, and 2009,28(11), and 88] need not sample is carried out derivatization, pre-treatment is quick, easy, and detection sensitivity is high, and resolution characteristic is strong.Therefore, be the more efficiently detection method of pentachlorophenol.
Summary of the invention:
Purpose of the present invention just is being based on above-mentioned current condition and the assay method of In Determination of Residual Pentachlorophenol in a kind of cigarette paper using of providing, this method has overcome the prior art defective, can fast, accurately detect pentachloro-phenol residual quantity in the paper, and measurement result is accurate, mensuration is disturbed few.
The objective of the invention is to be achieved through the following technical solutions:
The assay method of In Determination of Residual Pentachlorophenol in a kind of cigarette paper using is that the cigarette paper using is shredded rear adding extract, then ultrasonic extraction, and extract is centrifugal rear directly with the method for pentachloro-phenol residual quantity in the liquid chromatography tandom mass spectrometry determination paper, specifically may further comprise the steps:
A, cigarette paper using sample is carried out cutting according to relevant regulations: the cutting method of cigarette tipping paper carries out according to the regulation of YC 171-2008, namely accurately cuts long 200 mm, the tipping paper sample of wide 40 mm (should comprise monolateral); The cutting method of tobacco lining paper carries out according to the regulation of YC 264-2008, i.e. about 170 cm of cutting area
2(namely being equivalent to the internal lining paper area that the soft box packing of regular-size cigarette adopts); The cutting method of tobacco shred and box packaging paper carries out according to the regulation of YC/T 207-2006, namely to rigid pack paper, accurately cut the master package face with reference to the printing impression, area is 22.0 cm ', 5.5 cm, to soft box packaging paper, gets a soft box packaging paper, area is 15.5 cm ', 10.0 cm, to the bar wrapping paper, at packing front middle section, accurately cut the sample of 22.0 cm ', 5.5 cm;
The extraction of b, sample: the sample after the cutting placed on the balance take by weighing (being accurate to 0.01 g); Then sample is cut into the fragment that is not more than 0.5 cm * 0.5 cm with scissors; Fragment is placed 50 mL tool plug triangular flasks, accurately add 40mL extract (methyl alcohol: water=50:50, volume ratio) and 50 μ L inner mark solutions (2,4,5-T or 2,4-drip, concentration 1.0 μ g/mL), ultrasonic extraction 30 min;
C, sample purification: leave standstill 5 min, pipette extract 8 mL in 10 mL centrifuge tubes, with centrifugal 10 min of 10000 rpm speed.Draw supernatant, through 0.22 μ m organic phase membrane filtration, filtrate is detected through LC-MS/MS;
D, prepare standard operation solution: take by weighing respectively 0.01g(PCP) standard items are in the 10mL volumetric flask, with the methyl alcohol dilution and finally be mixed with the standard operation solution with concentration gradient;
E, liquid chromatography tandom mass spectrometry determination: draw the pesticide standard working solution of the variable concentrations for preparing, inject liquid chromatography-tandem mass spectrometer;
The calculating of f, In Determination of Residual Pentachlorophenol measurement result
Carry out quantitative test with internal standard method, namely with pentachlorophenol and interior target quota ion peak area is carried out regretional analysis to its respective concentration, obtain typical curve, related coefficient is more than or equal to 0.999, sample after extracting is measured, record and detect pentachlorophenol and interior target quota ion to peak area ratio, the substitution typical curve is tried to achieve the residual quantity of the pentachlorophenol in the sample.
The manner of formulation of standard operation solution is as follows in the present invention: take by weighing 0.01g PCP standard items to 100 mL volumetric flasks in, be accurate to 0.0001g, dilute constant volume with methyl alcohol, be mixed with the standard reserving solution that concentration is about 100 μ g/mL; Pipette standard reserving solution 1mL in the 100mL volumetric flask, dilute constant volume with methyl alcohol, obtain the working solution that concentration is about 1 μ g/mL; Pipette respectively the working solution of certain volume in 50 mL volumetric flasks, and add 50 μ L inner mark solutions (2,4,5-T, 1.0 μ g/mL).Dilute constant volume with methyl alcohol, namely be mixed with the pesticide standard working solution of variable concentrations, series standard working solution concentration is respectively: 2 ng/mL, 4 ng/mL, 6 ng/mL, 10 ng/mL, 20 ng/mL and 40 ng/mL;
The liquid phase chromatogram condition that adopts is: chromatographic column: Atiantis dC18 (150 mm * 2.1 mm, 3 μ m, U.S. Waters company); Mobile phase: acetonitrile/0.1 % aqueous formic acid (volume ratio 95:5), flow velocity: 200 μ L/min; Column temperature: 30 ℃; Sample size: 5 μ L; The mass spectrum condition that adopts: scan mode: negative ion scanning; Electric spray ion source (ESI); The atomization gas flow is 60 psi; Gas curtain airshed 18 psi; The auxiliary heating airshed is 60 psi; 500 ℃ of ionization temperature; The collision airshed is 10 psi; 4 kinds of gases are nitrogen; The residence time is 100 msec; Ionization voltage 5500 V, detection mode: negative ion polyion reaction monitoring (MRM), the MRM parameter sees Table 1.
Method of the present invention has overcome the deficiency of prior art sample treatment, has optimized sample-pretreating method and instrument testing conditions for cigarette tipping paper, internal lining paper and tobacco shred and box packaging paper sample.Compared with prior art the inventive method has following excellent results:
(1) the present invention takes pretreatment mode that sample is shredded, makes solvent better contact sample, and experimental result shows, processing can improve the extraction efficiency of pentachlorophenol like this.
(2) the inventive method utilizes LC-MS/MS to measure the content of pentachlorophenol in the paper, need not to carry out the derivatization operation, and pre-treating method is simple.
(3) the inventive method has advantages of accurate, the highly sensitive and good reproducibility of operation.
1. the detectability of the inventive method:
The pentachloro-phenol standard operation solution of variable concentrations is injected LC-MS/MS, calculate detectability (LOD) with 3 times of signal to noise ratio (S/N ratio)s (S/N=3), detect and be limited to 0.005 μ g/g.
2. the repeatability of the inventive method and recovery of standard addition:
Then the standard solution that adds pentachloro-phenol in blank sample carries out respectively pre-treatment and LC-MS/MS and analyzes, and calculate its recovery according to adding the scalar sum measured value, the results are shown in Table 2.As can be seen from Table 2, the recovery of pentachloro-phenol reaches more than 95%, and average relative standard deviation (RSD) illustrates that the recovery of the inventive method is high, good reproducibility less than between 5%.
Description of drawings
Fig. 1 is assay method process flow diagram of the present invention (this figure is as Figure of abstract).
Embodiment
The present invention is described further below in conjunction with example, but is not restriction the present invention.
Example 1:
1. instrument and reagent:
Pentachlorophenol, methyl alcohol, acetic acid are chromatographic grade reagent; Distilled water meets the requirement of one-level water among the GB/T 6682.
API 4000 quadrupole rod tandem mass spectrometers; Switzerland Mettler AE 163 electronic balance (sensibility reciprocals: 0.0001g).
2. sample preparation:
First sample is carried out cutting: the cutting method of cigarette tipping paper carries out according to the regulation of YC 171-2008, namely accurately cuts long 200 mm, the tipping paper sample of wide 40 mm (should comprise monolateral); Sample after the cutting is placed weighing on the balance; Then sample is cut into the fragment that is not more than 0.5 cm * 0.5 cm with scissors; Fragment is placed 50 mL tool plug triangular flasks, accurately add 40mL extract and 50 μ L inner mark solutions (2,4,5-T, 1.0 μ g/mL), ultrasonic extraction 30 min; Leave standstill 5min, get 8 mL supernatant liquors in 10 mL tool plug centrifuge tubes, centrifugal 10 min of 10000 rotary speeds, getting supernatant is liquid to be measured;
3. prepare standard operation solution: take by weighing 0.01g PCP standard items to 100 mL volumetric flasks in, be accurate to 0.0001g, dilute constant volume with methyl alcohol, be mixed with the standard reserving solution that concentration is about 100 μ g/mL; Pipette standard reserving solution 1mL in the 100mL volumetric flask, dilute constant volume with methyl alcohol, obtain the working solution that concentration is about 1 μ g/mL; Pipette respectively the working solution of certain volume in 50 mL volumetric flasks, and add 50 μ L inner mark solutions (2,4,5-T, 1.0 μ g/mL).Dilute constant volume with methyl alcohol, namely be mixed with the pesticide standard working solution of variable concentrations, series standard working solution concentration is respectively: 2 ng/mL, 4 ng/mL, 6 ng/mL, 10 ng/mL, 20 ng/mL and 40 ng/mL;
4. assay method: carry out quantitative test with internal standard method, namely with pentachlorophenol and interior target quota ion peak area is carried out regretional analysis to its respective concentration, obtain typical curve, related coefficient is more than or equal to 0.999, sample after extracting is measured, record and detect pentachlorophenol and interior target quota ion to peak area ratio, substitution typical curve, the content of trying to achieve the pentachloro-phenol in this tipping paper sample are respectively 0.05 μ g/g.
Accuracy for determination methods, the pentachlorophenol standard solution that in this sample, adds 0.05 μ g, carry out the same sample pre-treatments, record the selection quasi-molecular ions area of pentachlorophenol with LC-MS/MS, the substitution typical curve, the pentachlorophenol content of trying to achieve in sample this moment is 0.096 μ g/g, and namely the recovery of standard addition of pentachlorophenol is 96.0%, illustrates that the method is accurately.
Example 2:
As described in Example 1, select another cigarette tipping paper sample, record that pentachlorophenol content is 0 in the sample.
Example 3:
As described in Example 1, select another tobacco lining paper sample, the content that records pentachlorophenol in the sample is 0.
Claims (6)
1. the assay method of In Determination of Residual Pentachlorophenol in the cigarette paper using, it is characterized in that: be that the cigarette paper using is shredded rear adding extract, then ultrasonic extraction, extract is centrifugal rear directly with the method for pentachloro-phenol residual quantity in the liquid chromatography tandom mass spectrometry determination paper, specifically may further comprise the steps:
A, cigarette paper using sample is carried out cutting according to relevant regulations;
The extraction of b, sample: the sample after the cutting placed on the balance take by weighing (being accurate to 0.01 g); Be cut into fragment; Fragment is placed 50 mL tool plug triangular flasks, accurately add 40mL extract and 50 μ L inner mark solutions, ultrasonic extraction 30 min, extract are methyl alcohol: water=50:50, volume ratio;
C, sample purification: leave standstill 5 min, pipette extract 8 mL in 10 mL centrifuge tubes, with centrifugal 10 min of 10000 rpm speed; Draw supernatant, through 0.22 μ m organic phase membrane filtration, filtrate is detected through LC-MS/MS;
D, preparation standard operation solution: take by weighing respectively 0.01g pentachlorophenol standard items in 10 mL volumetric flasks, also finally be mixed with the standard operation solution with concentration gradient with the methyl alcohol dilution;
E, liquid chromatography tandom mass spectrometry determination: draw the pesticide standard working solution of the variable concentrations for preparing, inject liquid chromatography-tandem mass spectrometer;
The calculating of f, In Determination of Residual Pentachlorophenol measurement result
Carry out quantitative test with internal standard method, namely with pentachlorophenol and interior target quota ion peak area is carried out regretional analysis to its respective concentration, obtain typical curve, related coefficient is more than or equal to 0.999, sample after extracting is measured, record and detect pentachlorophenol and interior target quota ion to peak area ratio, the substitution typical curve is tried to achieve the residual quantity of the pentachlorophenol in the sample.
2. the assay method of In Determination of Residual Pentachlorophenol in the cigarette paper using according to claim 1, it is characterized in that: described inner mark solution is that 2,4,5-T or 2,4-drip, and concentration is 1.0 μ g/mL.
3. the assay method of In Determination of Residual Pentachlorophenol in the cigarette paper using according to claim 1, it is characterized in that: described cigarette paper using is tobacco lining paper, tipping paper, bar box packaging paper.
4. the assay method of In Determination of Residual Pentachlorophenol in the cigarette paper using according to claim 1, it is characterized in that: the relevant regulations among the step a refers to: the cutting method of cigarette tipping paper carries out according to the regulation of YC 171-2008, namely accurately cut long 200 mm, the tipping paper sample of wide 40 mm, should comprise one monolateral; The cutting method of tobacco lining paper carries out according to the regulation of YC 264-2008, i.e. about 170 cm of cutting area
2, namely be equivalent to the internal lining paper area that the soft box packing of regular-size cigarette adopts; The cutting method of tobacco shred and box packaging paper carries out according to the regulation of YC/T 207-2006, namely to rigid pack paper, accurately cut the master package face with reference to the printing impression, area is 22.0 cm ', 5.5 cm, to soft box packaging paper, gets a soft box packaging paper, area is 15.5 cm ', 10.0 cm, to the bar wrapping paper, at packing front middle section, accurately cut the sample of 22.0 cm ', 5.5 cm.
5. the assay method of In Determination of Residual Pentachlorophenol in the cigarette paper using according to claim 1, it is characterized in that: take by weighing 0.01g PCP standard items to 100 mL volumetric flasks in, be accurate to 0.0001g, dilute constant volume with methyl alcohol, be mixed with the standard reserving solution that concentration is about 100 μ g/mL; Pipette standard reserving solution 1mL in the 100mL volumetric flask, dilute constant volume with methyl alcohol, obtain the working solution that concentration is about 1 μ g/mL; Pipette respectively the working solution of certain volume in 50 mL volumetric flasks, and add 50 μ L inner mark solutions, dilute constant volume with methyl alcohol, namely be mixed with the pesticide standard working solution of variable concentrations, series standard working solution concentration is respectively: 2 ng/mL, 4 ng/mL, 6 ng/mL, 10 ng/mL, 20 ng/mL and 40 ng/mL.
6. the assay method of In Determination of Residual Pentachlorophenol in the cigarette paper using according to claim 1, it is characterized in that: the liquid phase chromatogram condition of employing is: chromatographic column: Atiantis dC18, specification 150 mm * 2.1 mm, 3 μ m; Mobile phase: acetonitrile/0.1 % aqueous formic acid, volume ratio 95:5, flow velocity: 200 μ L/min; Column temperature: 30 ℃; Sample size: 5 μ L; The mass spectrum condition that adopts: scan mode: negative ion scanning; Electric spray ion source (ESI); The atomization gas flow is 60 psi; Gas curtain airshed 18 psi; The auxiliary heating airshed is 60 psi; 500 ℃ of ionization temperature; The collision airshed is 10 psi; 4 kinds of gases are nitrogen; The residence time is 100 msec; Ionization voltage 5500 V, detection mode: negative ion polyion reaction monitoring (MRM).
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| CN104820053A (en) * | 2015-05-06 | 2015-08-05 | 宁波市海洋与渔业研究院 | Method of measuring nineteen chloro-phenols and sodium salt thereof in aquatic animals through gas chromatography-mass spectrography (GC-MS) method |
| CN108872336A (en) * | 2018-06-22 | 2018-11-23 | 上海烟草集团有限责任公司 | A kind of detection method for pentachlorophenol content in paper wrapper |
| CN113281287A (en) * | 2021-05-18 | 2021-08-20 | 福建中烟工业有限责任公司 | Paper surface layer pretreatment method and method for measuring content of saccharin sodium in paper surface layer |
| CN115508470A (en) * | 2022-09-21 | 2022-12-23 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | Method for detecting pentachlorophenol content in milk powder |
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| CN104820053A (en) * | 2015-05-06 | 2015-08-05 | 宁波市海洋与渔业研究院 | Method of measuring nineteen chloro-phenols and sodium salt thereof in aquatic animals through gas chromatography-mass spectrography (GC-MS) method |
| CN108872336A (en) * | 2018-06-22 | 2018-11-23 | 上海烟草集团有限责任公司 | A kind of detection method for pentachlorophenol content in paper wrapper |
| CN113281287A (en) * | 2021-05-18 | 2021-08-20 | 福建中烟工业有限责任公司 | Paper surface layer pretreatment method and method for measuring content of saccharin sodium in paper surface layer |
| CN113281287B (en) * | 2021-05-18 | 2023-10-31 | 福建中烟工业有限责任公司 | Pretreatment method for paper surface layer and method for determining saccharin sodium content in paper surface layer |
| CN115508470A (en) * | 2022-09-21 | 2022-12-23 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | Method for detecting pentachlorophenol content in milk powder |
| CN115508470B (en) * | 2022-09-21 | 2023-05-30 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | Method for detecting pentachlorophenol content in milk powder |
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