CN101650348B - Method for detecting safety limit of dissolution type fabric antibacterial bacteriostatic agent - Google Patents
Method for detecting safety limit of dissolution type fabric antibacterial bacteriostatic agent Download PDFInfo
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Abstract
The invention discloses a method for detecting the safety limit of a dissolution type fabric antibacterial bacteriostatic agent, which is characterized by comprising the following steps: (1) selecting a dissolution type fabric antibacterial bacteriostatic agent target compound; (2) detecting the residual of the dissolution type fabric antibacterial bacteriostatic agent target compound; and (3) detecting the dissolution migration of the dissolution type fabric antibacterial bacteriostatic agent target compound under the conditions of simulated body fluid and soaping. The method can apply safety limit detection and product safety assessment of alpha-bromation cinnamaldehyde of the dissolution type antibacterial finishing agent in antibacterial fabrics.
Description
Technical field
The invention belongs to product safety and detection technique field, be specifically related to a kind of threshold limit values assay method of dissolution type fabric antibacterial bacteriostatic agent.
Background technology
Along with science and technology development, textile satisfy people keep out the cold hide the primary demand of body after, expand out other functions gradually.Antibiotic fabrics such as all kinds of antibacterial underwears, antibiotic socks, antimicrobial yarn, antibacterial medical textile, moist antibacterial towel are just becoming the hot item on the market.So-called antibiotic fabric is meant under the prerequisite that does not change sense organ of fabric own or physical and chemical character (like intensity, water absorptivity, feel, aberration); Use various antiseptics that fabric is carried out antibiotic processing; Not only make fibrous material itself can resist microorganism and decompose rottenly, also can make attached to microorganism devitalization on the fabric or excessive multiplication not.At present the job operation of antibiotic fabric mainly contains two kinds, and a kind of is directly to adopt anti-bacterial fibre to process each kind fabric, and another kind is fabric to be carried out antibiotic finish process and obtain anti-microbial property.
Antimicrobial technology makes fabric obtain new function, but the antimicrobial technology improper use also possibly bring potential security hidden danger." about chemicals registration, assessment, permission and the restrictive system " that on Dec 18th, 2006, parliament of European Union and EU Council formally passed through jointly (being called for short the REACH instruction) is used to guarantee at present 30,000 kinds of chemicals compliance with environmental protection requirements of use in the world; The spy of European Union has set up the enforcement of European chemicals management board to guarantee that REACH instructs, and all chemical substances that get in European Union markets all need be in this management board's registration.Because of the constraint of REACH instruction and the enforcement of ecological textile standard, the antibacterial finishing agent security of on textile, widely using need be re-recognized, and gives necessary risk assessment.Although still there is not the mandatory security legislation of antibiotic textile at present; Seeing that the quality defect of antibacterial fabric possibly cause the substance harm to the public; And similar REACH instruction has clear and definite use restriction to the chemical substance of textile trade in the reality; When carrying out the antibacterial fabric assessment of function, paying close attention to its security is very important; Can not ignore environment and healthy safety in order to pursue antibacterial effect simply, especially should not carry out antibacterial treatment being applicable to textile and articles for use that the baby is correlated with.
The safety evaluatio of antibiotic fabric mainly is the burst size of antibacterial finishing agent in the repeatedly patch test, and the control of limiting the quantity of of elution amount in the test of perspiration resistance, colour fastness to washing.Often need carry out the extraction and the purification of target compound in kind liquid earlier to the residual said determination that carries out of the antibacterial finishing agent in the fabric sample; Then according to the characteristic of component to be measured; Adopt vapor-phase chromatography or high performance liquid chromatography to separate, select suitable highly sensitive selective detector to detect.
Antibacterial finishing agent retention analysis sample pre-treatments technology commonly used can have liquid-liquid extraction, SPE, Microwave Extraction, ultrasonic Extraction, ion-exchange etc.; Method for concentration has K-D concentrator concentration method, rotary evaporation in vacuo method etc., and the similar sample handling procedure often occupies a large amount of experimental periods.According to statistics, the time that sample pre-treatments spent accounts for 61% of The whole analytical process.The pre-treatment new technology of textile poisonous and harmful substance retention analysis in the recent period has been not limited to methods such as SPE (SPE), SPME (SPME), microwave auxiliary extraction (MAE), Suo Shi extractions automatically, online HPLC extraction, has similarly become the focus in the poisonous and harmful substance multi-residue analysis in the consumer goods from new technologies such as hydrodynamic-liquid distribution, accelerated solvent extraction (ASE), gel permeation chromatography (GPC), purging distillation technique (PT), supercritical fluid extraction (SFE), matrix solid phase dispersion extraction (MSPDE), molecular engram synthesis of receptor (MISR), immune affinity chromatographic columns.Yet the organic antibacterial agent that has volatilization or distillation characteristic because of market is used is a lot, can't total number contain wherein, detects the desk study stage that also is in as textile organic anti-bacterial bacteriostatic agent threshold limit values.The present invention comes therefrom.
Summary of the invention
The object of the invention is to provide a kind of threshold limit values assay method of dissolution type fabric antibacterial bacteriostatic agent, has solved that antibiotic fabric threshold limit values detection method lacks problems such as the safety evaluatio that causes antibiotic fabric can't carry out in the prior art.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of threshold limit values assay method of dissolution type fabric antibacterial bacteriostatic agent is characterized in that said method comprising the steps of:
(1) selects dissolution type fabric antibacterial bacteriostatic agent target compound;
(2) residual quantity of detection dissolution type fabric antibacterial bacteriostatic agent target compound;
(3) detect the stripping migration amount of dissolution type fabric antibacterial bacteriostatic agent target compound under the simulated body fluid and the condition of soaping.
Preferably, target compound is an alpha-bromo-cinnamaldehyde in the said step (1).
Preferably, the residual quantity of dissolution type fabric antibacterial bacteriostatic agent target compound detects through following method in the said step (2):
Accurately take by weighing after shredding sample and the anhydrous sodium sulfate crossed of acidification fully mix; Put into the extraction sleeve pipe through filling funnel; Extracting tube is placed in instrument or the automatic sampling dish; After the solvent extraction all extracts purify the back evaporation and concentration near dried through solid-phase extraction device, with the methylene chloride constant volume, through GC/MS analyze antibiotic bacteriostat target compound total amount.
Preferably, quick solvent extraction method is adopted in said solvent extraction, and said solvent is a methyl alcohol.
Preferably, the condition of solvent extraction method is fast: system pressure: 10Mpa; Temperature: 80 ℃; Heat time heating time: 2min; Stabilization time: 5min; Scavenging period: 1min; Flush volume: 100% abstraction pool volume; The nitrogen purging time: 1min.
Preferably, the detection method of stripping migration amount is following in the said step (3):
Accurately take by weighing sample after shredding in sample bottle, add the ultrasonic auxiliary extraction of leaching liquor under the simulated body fluid or the condition of soaping, the extract that obtains through solid-phase extraction device purify, enrichment, evaporation and concentration is done near, the methylene chloride constant volume supplies GC/MS to analyze; Get distilled water simultaneously and operate, as sample blank, supply GC/MS to analyze with this by above-mentioned same program; Obtain the stripping migration amount of target compound under the different condition.
Preferably, described leaching liquor is selected from simulate saliva, simulation acidic sweat and soap lye respectively.
Preferably, said solid-phase extraction device decontaminating column elution requirement is: eluting solvent is a methylene chloride, and eluting solvent consumption 10mL divides three drip washing.
Preferably, the condition determination of said GC/MS analytical approach is: chromatographic column: 15m * 0.25 μ m * 0.25mm HP-5; Injector temperature: 250 ℃; Input mode: split sampling not; Sample size: 1 μ L; Flow rate of carrier gas: 1.0ml/min (He); Temperature programme: 80 ℃ (2min), keeps 3min by 20 ℃/min to 260 ℃; Interface temperature: 280 ℃; Ion gun: electron bombardment ionization source; Multiplier electrode: 1880Volt; Sweep limit: 50-700amu; Select ionic means quantitative with molecular ion peak; Tuning manner: automatically.
It is target compound that method of the present invention is chosen with the alpha-bromo-cinnamaldehyde; Set up the method for detecting residue of antibacterial fabric dissolution type antibacterial finishing agent alpha-bromo-cinnamaldehyde; Confirm the stripping migration amount of target compound under the different condition; Observe the security of the stripping quantity (migration amount) under specific condition with further research, thereby set up the secure threshold in system of alpha-bromo-cinnamaldehyde hazard assessment accurately and the rational textile.
With respect to scheme of the prior art, advantage of the present invention is:
The present invention has set up the organic extractant phase of dissolution type antibacterial finishing agent alpha-bromo-cinnamaldehyde in the suitable textile and the technical program of the ultrasonic auxiliary extraction of simulated body fluid; In conjunction with of enrichment, the purification of preferred
solid-phase extraction device to extract; Carry out the qualitative and quantitative analysis of target compound by gas chromatography-mass spectrum, measure applicable to dissolution type antibacterial finishing agent alpha-bromo-cinnamaldehyde total amount and simulated body fluid stripping quantity in all kinds of textiles such as clothes, fiberfill, yarn, dress materials and home decoration product.This invention has that consumption of organic solvent is few, rate of extraction is fast, impurity disturbs less, the high outstanding advantage of sample recovery rate; And can be residual through alpha-bromo-cinnamaldehyde total amount in the sample and the difference of stripping quantity, more accurately set up alpha-bromo-cinnamaldehyde hazard assessment system and reasonable security health threshold value.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further described:
Fig. 1 is the total ion current figure (TIC) of target compound alpha-bromo-cinnamaldehyde reference material;
Fig. 2 is the gas chromatography-mass spectrum figure of target compound alpha-bromo-cinnamaldehyde reference material;
Fig. 3 is actual sample total ion current figure (TIC figure);
Fig. 4 is a target compound alpha-bromo-cinnamaldehyde typical curve.
Embodiment
Below in conjunction with specific embodiment such scheme is further specified.Should be understood that these embodiment are used to the present invention is described and are not limited to limit scope of the present invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
Alpha-bromo-cinnamaldehyde detects in the embodiment antibiotic fabric
Material and method
1, instrument and reagent:
Branson 200ULTRASONIC Cleaner (frequency 48kHz, power 50Watt); 5975/6890 gas chromatograph-mass spectrometer (GCMS), Angilent
TMCompany; HP-5 (30m * 0.25mm * 0.25 μ m), Angilent
TMCompany; The quick solvent extraction appearance of Dionex.ASE200 (join the 11mL abstraction pool, fibre abstraction is used sleeve pipe); Supelco SPE solid-phase extraction device: SUPELCO Visiprep
TMDL 12 hole solid-phase extraction devices; The BOA-P504-BN type does not have oily vacuum diaphragm pump; Methyl alcohol (Methanol, HPLC level), AH230-4, Honeywell Burdick & Jackson, USA; Methylene chloride (DCM, HPLC level), L2232049, Accustandard
TM, USA; Alpha-bromo-cinnamaldehyde (Alpha-Bromocinnamaldehyde, BCA), L22787098, Accustandard
TM, USA; Helium: purity 99.999%; Nitrogen: purity 99.999%; Standard is pasted lining: cotton standard is pasted lining (ISO 105-F09); Artificial saliva (Solution I): take by weighing sodium chloride (2.5.18) 0.5g, soda mint (2.5.19) 4.2g, sal tartari (2.5.20) 0.2g is dissolved in the 1L water; Artificial acidic sweat (Solution II): get L-histidine hydrochloride (2.5.21) 0.5g; Sodium chloride (2.5.18) 5g; Hypophosphite monohydrate sodium dihydrogen (2.5.22) 2.2g, the HCl solution (2.5.25) of 0.01mol/L and 0.01mol/L NaOH (2.5.26) are transferred pH5.5, join existing usefulness at present; Soap lye: contain in every premium on currency (annotate: this is three grades of water, meets GB/T6682-1992): 5g soap (meeting GB/T 3921-2008 requires); Solid-phase extraction device pre-filled pillar: Supelclean
TM 
Solid-phase extraction device Tube or suitable person, Supelco
TMCompany.
2, instrument condition
Set the instrumental analysis condition: chromatographic column: 15m * 0.25 μ m * 0.25mm HP-5; Injector temperature: 250 ℃; Input mode: split sampling not; Sample size: 1 μ L; Flow rate of carrier gas: 1.0ml/min (He); Temperature programme: 80 ℃ (2min), keeps 3min by 20 ℃/min to 260 ℃; Interface temperature: 280 ℃; Ion gun: electron bombardment ionization source; Multiplier electrode: 1880Volt; Sweep limit: 50-700amu; Select ionic means quantitative with molecular ion peak; Tuning manner: atune.
3, alpha-bromo-cinnamaldehyde assay determination
Accurately take by weighing the 0.5g sample; Shred to 2.5mm * 2.5mm; The anhydrous sodium sulfate of crossing with 0.5g acidification fully mixes the back and puts into extraction sleeve pipe (11mL) through filling funnel, and extracting tube is placed instrument or automatically in the sampling dish, the solvent extraction appearance begins to extract by the program parameter of setting fast: inject methyl alcohol to abstraction pool; With abstraction pool heating and pressurization; Keep sample static extracting under the pressure and temperature of setting, pump is seen extract in the abstraction pool off, with the nitrogen purging sample to obtain whole extracts.Purify the final vacuum rotary evaporation through
solid-phase extraction device and concentrate near doing; Methylene chloride is settled to 1mL; Supply GC/MS to analyze, obtain the total amount of target compound in the sample.
Quick solvent extraction appearance operating conditions: system pressure: 10Mpa; Temperature: 80 ℃; Heat time heating time: 2min; Stabilization time: 5min; Scavenging period: 1min; Flush volume: 100% (abstraction pool volume); The nitrogen purging time: 1min.
Accurately take by weighing 0.5g and shred sample, place in the 22mL sample bottle to 2.5mm * 2.5mm.Add 10mL leaching liquor (artificial saliva, artificial acidic sweat, soap lye); Bottle stopper with being lined with the polytetrafluoroethylene (PTFE) dottle pin seals; Behind the ultrasonic auxiliary extraction 30min, cooling is after
solid-phase extraction device purifies, enrichment, simultaneously with 2 * 3mL methanol wash receiving flask; Cleaning solvent is crossed post in the lump; Divide three drip washing with the 10mL methylene chloride after leaving standstill 10min, 50 ℃ of rotary evaporation in vacuo of leacheate are concentrated near doing, methylene chloride is settled to 1mL; Transfer to automatic sampler with in the sample bottle, air feed matter combined instrument GC/MS analyzes.Get 10mL distilled water simultaneously and operate by above-mentioned same program, with this as sample blank.
3.1 the foundation of alpha-bromo-cinnamaldehyde calibration curve
The drafting of calibration curve: prepare calibration standard series solution by the alpha-bromo-cinnamaldehyde standard reserving solution: 10; 20; 40,60,100 μ g/L; Join respectively in the clean 15mL sample bottle; Add the known standard subsides lining that does not contain target compound that 0.5g shreds again, carry out accelerated solvent extraction then, concentrate closely through
solid-phase extraction device purification final vacuum rotary evaporation and do; Methylene chloride is transferred to automatic sampler with in the sample bottle after being settled to 1mL, carries out GC/MS with 1 μ L sample size and analyzes.Other gets some and has added blank cotton standard that 0.5g shreds and paste lining and carry out blank replicate determination.After deducting the blank value of identical sample size, obtain the linear relationship of the concentration of target compound to response (chromatogram peak height).
Typical curve is a horizontal ordinate with the concentration (mg/L) of target compound to be measured, and measured value (peak area) is an ordinate production standard curve, confirms the range of linearity, gets the compound amount of five concentration point and carries out PLS, obtains regression equation.The amount of target compound and the amount of the recovery adopt same equation to calculate.The detectability of instrument (LODs) is defined as 3 times of signal-to-noise ratios, and (3 * S/N), instrument is 0.001ng/g to alpha-bromo-cinnamaldehyde, and in the range of linearity of determining, method is limited to 0.005mg/kg to the minimum detection of alpha-bromo-cinnamaldehyde in the actual sample, sees table 1.
Table 1 alpha-bromo-cinnamaldehyde is linear limits the quantity of with detection
3.2 blank mark-on and matrix (cotton standard is pasted lining) recovery of standard addition is measured
Employing method blank controls whether pollution artificial or that environmental factor is brought is arranged in the whole experiment in the experimentation, is adopting the blank accuracy of coming (in zero standard card lining, adding target compound) the confirmatory experiment process of matrix mark-on near the detectability.With the target compound standard solution preparation standard sample of concentration 5ng/mL, 20ng/mL, 100ng/mL, carry out recovery test, do blank test with the sample of identical material in addition, measure the result and see table 2.Blank recovery of standard addition is at 94.5-102.5%, and RSD is 2.2-4.9%, and the matrix recovery of standard addition is at 92.6-97.5%, and RSD is 3.1-6.8%.
Blank mark-on of table 2 and matrix (cotton standard is pasted lining) recovery of standard addition is measured the result
Analyze containing target compound standard operation liquid by the instrumental analysis condition, adopt and select ion detection (SIM) mode that its characteristic ion signal is gathered, gained chromatogram and retention time are seen Fig. 2.
To the fabric sample alpha-bromo-cinnamaldehyde stripping migration that contains the alpha-bromo-cinnamaldehyde antibacterial finishing agent, it is sample substrate that research is pasted lining with cotton standard, adds the target method through blank, has compared the stripping influence of different extracts to the alpha-bromo-cinnamaldehyde stripping quantity.Experimental result is seen shown in the table 3.
Alpha-bromo-cinnamaldehyde in the cotton standard subsides of table 3 lining is in the migration amount of different extracts
It is thus clear that; As the dissolution type antibacterial finishing agent; Alpha-bromo-cinnamaldehyde has very high stripping quantity, with soap under the condition almost can both stripping, has both shown its antibiotic permanance poor effect at simulated body fluid; Confirm also that simultaneously this series products can continue to reach release wear use, exists the health risk of pungency and sensitization to skin.Based on the security consideration of European Union, when pursuing good antibacterial effect, should avoid the use of the so high stripping antibacterial finishing agent of similar BCA to the textile chemical substance.
Be the practicality of checking assay method to the detection of alpha-bromo-cinnamaldehyde in the antibacterial fabric; The alpha-bromo-cinnamaldehyde active component residual level that 35 kinds of antibiotic fabric finished products are carried out detects; Discovery detects target compound in 1 sample, between residual level 134 ± 3.62mg/kg, and simulate saliva stripping quantity 9.5 ± 1.01mg/kg; Simulate sour sweat stripping quantity 14.2 ± 5.1mg/kg, soap lye stripping quantity 23.5 ± 3.2mg/kg.It is thus clear that the environment and the healthy and safe property of the alpha-bromo-cinnamaldehyde that uses as antibacterial finishing agent should give concern.
This method is target compound with the alpha-bromo-cinnamaldehyde, and fabric sample is aided with the ultrasonic householder method of leaching liquor simultaneously through the methyl alcohol accelerated solvent extraction, has measured the residual and stripping quantity of target compound in the sample respectively with gas chromatograph-mass spectrometer GC/MS.Method is limited to 0.005mg/kg to the detection of target compound, and blank mark-on yield is at 94.5-102.5%, and RSD is 1.9-3.6%, and the matrix recovery of standard addition is at 92.6-97.5%, and RSD is 2.1-4.8%.This method combines " anti-family of GB/T 12490-1990 textile and commercial laundering colour fastness test method " or " home washings and the drying program that adopt during the test of ISO 6330-2000 textile " (ISO 6330 Textiles-Domestic washing and drying procedures fortextile testing) assessment procedure to fastness to washing; And the textile of mandatory national standard " GB18401-2008 country textile product basic security technical manual " regulation can be implemented threshold limit values to dissolution type antibacterial finishing agent alpha-bromo-cinnamaldehyde in the antibacterial fabric and detect and the product safety evaluation the harmless requirement of health.
Above-mentioned instance only is explanation technical conceive of the present invention and characteristics, and its purpose is to let the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (6)
1. the assay method of dissolution type fabric antibacterial bacteriostatic agent residual quantity and stripping migration amount is characterized in that said method comprising the steps of:
(1) with the alpha-bromo-cinnamaldehyde be dissolution type fabric antibacterial bacteriostatic agent target compound, detect the residual quantity of dissolution type fabric antibacterial bacteriostatic agent target compound through following steps:
Accurately take by weighing after shredding sample and the anhydrous sodium sulfate crossed of acidification fully mix; Put into the extraction sleeve pipe through filling funnel; Extracting tube is placed in instrument or the automatic sampling dish; After the solvent extraction all extracts purify the back evaporation and concentration near dried through solid-phase extraction device, with the methylene chloride constant volume, through GC/MS analyze antibiotic bacteriostat target compound total amount;
(2) with the alpha-bromo-cinnamaldehyde be dissolution type fabric antibacterial bacteriostatic agent target compound, detect the stripping migration amount of dissolution type fabric antibacterial bacteriostatic agent target compound under the simulated body fluid and the condition of soaping through following steps:
Accurately take by weighing sample after shredding in sample bottle, add the ultrasonic auxiliary extraction of leaching liquor under the simulated body fluid or the condition of soaping, the extract that obtains through solid-phase extraction device purify, enrichment, evaporation and concentration is done near, the methylene chloride constant volume supplies GC/MS to analyze; Get distilled water simultaneously and operate, as sample blank, supply GC/MS to analyze with this by above-mentioned same program; Obtain the stripping migration amount of target compound under the different condition.
2. method according to claim 1 is characterized in that quick solvent extraction method is adopted in solvent extraction in the said method step (1), and said solvent is a methyl alcohol.
3. method according to claim 1 is characterized in that the condition of quick solvent extraction method in the said method step (1) is: system pressure: 10Mpa; Temperature: 80 ℃; Heat time heating time: 2min; Stabilization time: 5min; Scavenging period: 1min; Flush volume: 100% abstraction pool volume; The nitrogen purging time: 1min.
4. method according to claim 1 is characterized in that leaching liquor is selected from simulate saliva, simulation acidic sweat and soap lye respectively in the said method step (2).
5. method according to claim 1, it is characterized in that said solid-phase extraction device decontaminating column elution requirement is: eluting solvent is a methylene chloride, eluting solvent consumption 10mL divides three drip washing.
6. method according to claim 1 is characterized in that the condition determination of said GC/MS analytical approach is: chromatographic column: 15m * 0.25 μ m * 0.25mm HP-5; Injector temperature: 250 ℃; Input mode: split sampling not; Sample size: 1 μ L; Flow rate of carrier gas: 1.0ml/min (He); Temperature programme: 80 ℃ (2min), keeps 3min by 20 ℃/min to 260 ℃; Interface temperature: 280 ℃; Ion gun: electron bombardment ionization source; Multiplier electrode: 1880Volt; Sweep limit: 50-700amu; Select ionic means quantitative with molecular ion peak; Tuning manner: automatically.
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| CN103760323A (en) * | 2014-01-09 | 2014-04-30 | 中华人民共和国苏州出入境检验检疫局 | Safety testing method for antibacterial textiles |
| US9783799B2 (en) * | 2014-10-24 | 2017-10-10 | Abbott Molecular Inc. | Enrichment of small nucleic acids |
| CN105223289B (en) * | 2015-09-14 | 2017-06-09 | 杭州市质量技术监督检测院 | The detection method of antiseptic in textile product |
| CN108445132A (en) * | 2018-03-26 | 2018-08-24 | 安徽回车服装有限公司 | A kind of textile chemistry method for detecting residue |
| CN110629565A (en) * | 2019-08-26 | 2019-12-31 | 徐州锦业纺织科技有限公司 | After-finishing process of rayon yarn |
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| Fang Zhu et al..Application of solid-phase microextraction for the determination of organophosphorus pesticides in textiles by gas chromatography with mass spectrometry.《Analytica Chimica Acta》.2009,第650卷(第9期),202-206. * |
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