CN104991003A - Method for measuring isothiazolinone antibacterial finishing agents in textiles - Google Patents
Method for measuring isothiazolinone antibacterial finishing agents in textiles Download PDFInfo
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Abstract
The invention provides a method for measuring isothiazolinone antibacterial finishing agents in textiles, and relates to the field of product quality analysis, and discloses a method for separating and detecting the five isothiazolinone antibacterial finishing agents. The following liquid phase chromatographic conditions are adopted, and according to the liquid phase chromatographic conditions, a chromatographic column is XR-ODS (2.2 microns), the inner diameter is 100 mm*3.0 mm, column temperature is 40 DEG C, column flow speed is 0.4ml/min, a diode array detector is adopted, and detection wavelengths are 277 nm and 283 nm. According to the gradient elution conditions, the volume ratio of methanol to water is 40 to 60 for 0.00 min; the volume ratio of methanol to water is 90 to 10 for 1.90 min; the volume ratio of methanol to water is 90 to 10 for 6.00 min; the volume ratio of methanol to water is 40 to 60 for 6.01 min; 9.00 min. The five isothiazolinone antibacterial finishing agents are separated, a good baseline separation effect can be achieved, and peak types are sharp and symmetric.
Description
Technical field
The present invention relates to product quality analysis field, be specifically related to the assay method of isothiazolinone antibacterial finishing agent in a kind of textile.
Background technology
OIT compounds is a kind of new type bactericide, has the advantages such as efficient, low toxicity, duration of efficacy are long, environmentally safe, causes the extensive concern of the experts such as biology, medicine, region of chemistry.Widespread use along with OIT compounds is anticorrosion at marine anti-pollution, industrial circulating cooling water process, industrial products, in agricultural bactericidal etc., the environmental behaviour of OIT compounds and eco-toxicity have caused the great attention of people, become the study hotspot in this field current.European Union cosmetics regulation 1223/2009 specifies and CMI and MI can use as antiseptic in stop class and flushing class cosmetics, and MI Cmax is 0.01% (100ppm) or the maximum solubility of CMI/MI (3:1) potpourri is 0.0015% (15ppm).European Union toy instruction EN71-9-2005 specifies MI, CMI, BIT content in toy leather, aqueous liquid, moulding clay, the material such as to tatoo containing the imitation of binder, its limitation is respectively 10,10 and 5mg/kg, and total limitation of MI and CMI is 15mg/kg.On April 21st, 2010, technical standard office of Korea S (KATS) issues No. G/TBT/N/KOR/270 circular, and " Consumer Product Safety standard proposals are " in the Permissible limit standard adding 10 kinds of harmful antiseptic products such as methylisothiazolinone, Phenoxyethanol, OIT of fabric softener.
Reported that the detection method of isothiazolinone antibacterial finishing agent is as follows at present: GB/T 29666-2013 " potpourri of Preservative Technology for Personal Care methylchloroisothiazandnone and methylisothiazolinone and magnesium chloride and magnesium nitrate ", what adopt in standard is that liquid phase chromatography is entered and oxidation-reduction method MI, CMI.Wherein specify, liquid phase chromatography is referee method.In liquid phase chromatography, chromatographic column used is C18 post, and mobile phase used is methanol/water.SN/T 2106-2008 " importing and exporting the mensuration liquid phase chromatography of methylisothiazolinone and chloro thing thereof in cosmetics ", what adopt in standard is that liquid phase chromatography measures MI, CMI, and chromatographic column used is C18 post, and mobile phase used is methanol/water." in toy, anticorrosion row measures SN/T 2404-2009, and chromatographic column used is C18 post, and mobile phase used is methanol/water.HG/T 3657-2008 " water treatment agent isothiazolinone derivatives ", standard adopts has two kinds of modes to measure MI, CMI, the mensuration of liquid phase chromatography agent MIT and derivant thereof respectively ", liquid phase chromatography is adopted to measure MI, CMI in standard, chromatographic column used is C18 post, and mobile phase used is methyl alcohol/0.4% acetic acid aqueous solution (volume fraction).EN 71-11 " toy safety organic compound: analytical approach ", adopts liquid phase chromatography to measure MI, CMI, BIT in standard, chromatographic column used is C18 chromatographic column, and mobile phase used is methyl alcohol/0.4% acetic acid aqueous solution (volume fraction).Yang Jingrong etc. adopt ultrasonic extraction, take methanol/water as mobile phase, MI, CMI, BIT in LC-MS/MS toy.
Not yet there is the detection method of thiazoline ketone antiseptic in textile at present, also do not have the method being simultaneously separated detection five kinds of quinoline ketone antiseptics.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, the detection method of isothiazolinone antibacterial finishing agent in textile is provided on the one hand; A kind of method being simultaneously separated detection 5 kinds of isothiazolinone antibacterial finishing agents is provided on the other hand.
In the context of the invention, MI is MIT, and CMI is the chloro-2 methyl-4-isothiazoline-3-ketone of 5-, BIT is 1,2-benzisothiazole-3-ketone, and OI is Kathon, DCOI is the chloro-Kathon of 4,5-bis-.
One aspect of the present invention provides the detection method of isothiazolinone antibacterial finishing agent in a kind of textile, and it comprises the following steps:
1) preparing standard solution: take 5 kinds of isothiazolinone antibacterial finishing agent standard items respectively, the Standard Stock solutions that concentration is 1000mg/L is mixed with respectively with extractant, pipette the Standard Stock solutions of isothiazolinone antibacterial finishing agent more respectively, be placed in volumetric flask, dilute with extractant and be settled to scale, shaking up;
2) testing sample solution is prepared
Testing sample is cut into the fragment of about 5mm × 5mm, mixing, then takes testing sample 1.0g, be placed in extractor, in extractor, add extractant extract, after being cooled to room temperature, extract is through the membrane filtration of 0.22um, and gained filtrate is for liquid chromatogram measuring;
3) liquid phase chromatogram condition
Chromatographic column is XR-ODS, and internal diameter is 100mm × 3.0mm; Flow velocity: 0.4mL/min; Column temperature: 40 DEG C; Detecting device: diode array detector (DAD); Determined wavelength: 277 ~ 319nm; Sample size: 1.0uL; Mobile phase A is methyl alcohol; Mobile phase B is water; Adopt gradient elution: time initial with 40% mobile phase A and 60% Mobile phase B, change the Mobile phase B of 90% mobile phase A and 10% in 2.0min internal linear, maintenance 4min; Then 0.5min internal linear changes the Mobile phase B of 40% mobile phase A and 60% into, keeps 4min;
4) drawing standard working curve
Get step 1) standard solution prepared, by step 3) liquid phase chromatogram condition sample introduction measures, take concentration of standard solution as horizontal ordinate, peak area is ordinate, drawing standard working curve;
5) measure
By pressing step 3) liquid phase chromatogram condition sample introduction mensuration, to step 2) testing sample solution prepared measures, the retention time of record chromatographic peak and peak area, qualitative according to the retention time of chromatographic peak, the peak area according to chromatographic peak carries out quantified by external standard method.
In step 1) in, described 5 kinds of isothiazolinone antibacterial finishing agents are MIT, the chloro-2 methyl-4-isothiazoline-3-ketone of 5-, 1,2-benzisothiazole-3-ketone, Kathon, 4,5-bis-chloro-Kathons;
In step 1) and step 2) in, described extractant can be selected from water, methyl alcohol, acetonitrile, normal hexane, acetone, ethyl acetate, t-butyl methyl ether etc., and in certain embodiments, described extractant is methyl alcohol, and the volume of described extractant is 20mL.
In step 2) in, described extractor can be selected from soxhlet's extractor, ultrasonic extraction device, microwave extracter etc., and in certain embodiments, described extractor is ultrasonic extraction device.
In step 2) in, the condition of described extraction is ultrasonic extraction 20min at 40 DEG C.
The present invention has following outstanding advantage:
Adopt method of the present invention effectively can extract 5 isothiazolinone antibacterial finishing agents in textile, thus ensure the reliability of testing result;
The present invention adopts high performance liquid chromatography/diode array detector method (HPLC-DAD) to carry out qualitative and quantitative analysis to isothiazolinone antibacterial finishing agent in textile, qualitative progress is easy, quantitative result is accurate, meets the demand importing and exporting textile and home market supervision.
The present invention not only easily operates, and precision and the recovery all meet the requirements, and can meet the testing requirement of isothiazolinone antibacterial finishing agent in textile.
The present invention provides a kind of method being simultaneously separated detection 5 kinds of isothiazolinone antibacterial finishing agents on the other hand, and it comprises the following steps:
1) preparation of hybrid standard working solution: take 5 kinds of isothiazoline class antibacterial finishing agent standard items respectively, 5 by 5 kinds of isothiazoline class antibacterial finishing agent standard items mixing, potpourri methyl alcohol is configured to the Standard Stock solutions that concentration is 1000mg/L, pipette the hybrid standard stock solution of 5 kinds of isothiazolinone antibacterial finishing agents, be placed in brown volumetric flask, be settled to scale with methanol dilution, shake up;
2) liquid phase chromatogram condition: XR-ODS (2.2 μm), internal diameter is 100mm × 3.0mm, column temperature is 40 DEG C, column flow rate is 0.4ml/min, adopt diode array detector, determined wavelength is respectively 277nm and 283nm, and when condition of gradient elution is initial, the volume ratio of methyl alcohol and water is 40:60; The volume ratio 90:10 that 1.90min internal linear changes methyl alcohol and water into keeps 6.00min; Change the volume ratio 40:60 of methyl alcohol and water during 6.01min into, keep 9.00min;
3) measure
By step 1) the hybrid standard working solution 1uL for preparing injects high performance liquid chromatograph, in step 2) carry out gradient elution under the liquid phase chromatogram condition that sets.
Described 5 kinds of isothiazolinone antibacterial finishing agents are MIT, the chloro-2 methyl-4-isothiazoline-3-ketone of 5-, 1,2-benzisothiazole-3-ketone, Kathon, 4,5-bis-chloro-Kathons.
5 kinds of isothiazolinone antibacterial finishing agents are successfully carried out separation and detect by the present invention, and 5 kinds of isothiazolinone antibacterial finishing agents can well reach baseline separation effect, and peak type is sharp-pointed, symmetrical.
Accompanying drawing explanation
Fig. 1 shows the HPLC chromatogram of OIT hybrid standard material under 277nm determined wavelength;
Fig. 2 shows the HPLC chromatogram of OIT hybrid standard material under 283nm determined wavelength.
Embodiment
In order to make those skilled in the art understand technical scheme of the present invention better, below disclose further some non-limiting embodiments the present invention is described in further detail.
The detection method of isothiazolinone antibacterial finishing agent in embodiment 1 textile
Reagent and material
Methyl alcohol: chromatographically pure.
5 kinds of OIT standard items: purity >=98%, 5 kinds of OIT standard items are respectively: MIT (being called for short MI), the chloro-2 methyl-4-isothiazoline-3-ketone of 5-(being called for short CMI), 1,2-benzisothiazole-3-ketone (being called for short BIT), Kathon (being called for short OI), 4,5-bis-chloro-Kathons (being called for short DCOI);
Detecting step is as follows:
(1) preparing standard solution: accurately take often kind of appropriate OIT standard items respectively, the Standard Stock solutions that concentration is 1000mg/L is mixed with respectively with methyl alcohol, pipette the Standard Stock solutions of 5 kinds of OITs of certain volume respectively, be placed in brown volumetric flask, be settled to scale with methanol dilution, shake up;
(2) testing sample solution is prepared
Testing sample is cut into the fragment of about 5mm × 5mm, mixing, then testing sample 1.0g is taken, be placed in 50mL ultrasonic extraction device, in ultrasonic extraction device, add 20mL methyl alcohol, the frequency of operation of setting ultrasonic extraction device is 40KHz, ultrasonic extraction 20min at 40 DEG C, after being cooled to room temperature, extract is through the organic phase pin type membrane filtration of 0.22um, and gained filtrate is for liquid chromatogram measuring;
(3) liquid phase chromatogram condition
A) chromatographic column: XR-ODS (2.2 μm), 100mm × 3.0mm (internal diameter);
B) flow velocity: 0.4mL/min;
C) column temperature: 40 DEG C;
D) detecting device: diode array detector (DAD);
E) determined wavelength: 190nm ~ 450nm;
F) quantitative wavelength: 277nm, 285nm, 319nm.
G) sample size: 1.0uL;
H) mobile phase A: methyl alcohol;
I) Mobile phase B: water;
J) gradient elution: time initial with 40% mobile phase A and 60% Mobile phase B, change the Mobile phase B of 90% mobile phase A and 10% in 2.0min internal linear, keep 4min; Then 0.5min internal linear changes the Mobile phase B of 40% mobile phase A and 60% into, keeps 4min.
(4) drawing standard working curve
Get the standard solution that (1) prepares, measure by (3) liquid phase chromatogram condition sample introduction, take concentration of standard solution as horizontal ordinate, peak area is ordinate, drawing standard working curve;
(5) measure
Measure by by (3) liquid phase chromatogram condition sample introduction, testing sample solution prepared by (2) is measured, the retention time of record chromatographic peak and peak area, qualitative according to the retention time of chromatographic peak, the peak area according to chromatographic peak carries out quantified by external standard method.
Embodiment 2 is separated the method for detection 5 kinds of isothiazolinone antibacterial finishing agents simultaneously
Step is as follows:
1) preparation of hybrid standard working solution: take 5 kinds of isothiazoline class antibacterial finishing agent standard items respectively, 5 by 5 kinds of isothiazoline class antibacterial finishing agent standard items mixing, potpourri methyl alcohol is configured to the Standard Stock solutions that concentration is 1000mg/L, pipette the hybrid standard stock solution of 5 kinds of isothiazolinone antibacterial finishing agents, be placed in brown volumetric flask, be settled to scale with methanol dilution, shake up;
2) liquid phase chromatogram condition: XR-ODS (2.2 μm), 100mm × 3.0mm (internal diameter), column temperature is 40 DEG C, column flow rate is 0.4ml/min, adopt diode array detector, determined wavelength is respectively 277nm and 283nm, and condition of gradient elution is 0.00min, methyl alcohol: water=40:60 (volume ratio); 1.90min, methyl alcohol: water=90:10 (volume ratio); 6.00min, methyl alcohol: water=90:10 (volume ratio); 6.01min, methyl alcohol: water=40:60 (volume ratio); 9.00min;
3) measure
By step 1) the hybrid standard working solution 1uL for preparing injects high performance liquid chromatograph, in step 2) carry out gradient elution under the liquid phase chromatogram condition that sets.
The Precision Experiment of embodiment 3 detection method
Choose positive cotton sample, numb sample, each portion of silk sample, carry out test 9 times respectively according to the method for embodiment 1, obtain the precision of method, all positive all measure OI, and concrete outcome is as shown in table 1:
The Precision Experiment of table 1 method
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the detection method of isothiazolinone antibacterial finishing agent in textile, is characterized in that it comprises the following steps:
1) preparing standard solution: take 5 kinds of isothiazolinone antibacterial finishing agent standard items respectively, the Standard Stock solutions that concentration is 1000mg/L is mixed with respectively with extractant, pipette the Standard Stock solutions of isothiazolinone antibacterial finishing agent more respectively, be placed in volumetric flask, dilute with extractant and be settled to scale, shaking up;
2) testing sample solution is prepared
Testing sample is cut into the fragment of about 5mm × 5mm, mixing, then takes testing sample 1.0g, be placed in extractor, in extractor, add extractant extract, after being cooled to room temperature, extract is through the membrane filtration of 0.22um, and gained filtrate is for liquid chromatogram measuring;
3) liquid phase chromatogram condition
Chromatographic column is XR-ODS, and internal diameter is 100mm × 3.0mm; B) flow velocity: 0.4mL/min; Column temperature: 40 DEG C; Detecting device: diode array detector (DAD); Determined wavelength: 277 ~ 319nm; Sample size: 1.0uL; Mobile phase A: methyl alcohol; Mobile phase B: water; Adopt gradient elution: time initial with 40% mobile phase A and 60% Mobile phase B, change the Mobile phase B of 90% mobile phase A and 10% in 2.0min internal linear, maintenance 4min; Then 0.5min internal linear changes the Mobile phase B of 40% mobile phase A and 60% into, keeps 4min;
4) drawing standard working curve
Get step 1) standard solution prepared, by step 3) liquid phase chromatogram condition sample introduction measures, take concentration of standard solution as horizontal ordinate, peak area is ordinate, drawing standard working curve;
5) measure
By step 3) liquid phase chromatogram condition sample introduction mensuration, to step 2) testing sample solution prepared measures, the retention time of record chromatographic peak and peak area, qualitative according to the retention time of chromatographic peak, the peak area according to chromatographic peak carries out quantified by external standard method.
2. detection method as claimed in claim 1, it is characterized in that in step 1) in, described 5 kinds of isothiazolinone antibacterial finishing agents are MIT, the chloro-2 methyl-4-isothiazoline-3-ketone of 5-, 1,2-benzisothiazole-3-ketone, Kathon, 4,5-bis-chloro-Kathons.
3. detection method as claimed in claim 1, in step 1) and step 2) in, described extractant is selected from water, methyl alcohol, acetonitrile, normal hexane, acetone, ethyl acetate, t-butyl methyl ether.
4. detection method as claimed in claim 3, is characterized in that described extractant is methyl alcohol.
5. the detection method as described in claim 1 or 4, is characterized in that the volume of described extractant is
20mL.
6. detection method as claimed in claim 1, is characterized in that in step 2) in, described extractor is selected from soxhlet's extractor, ultrasonic extraction device, microwave extracter.
7. detection method as claimed in claim 6, is characterized in that described extractor is ultrasonic extraction device.
8. detection method as claimed in claim 1, is characterized in that in step 2) in, the condition of described extraction is ultrasonic extraction 20min at 40 DEG C.
9. be separated a method for detection 5 kinds of isothiazolinone antibacterial finishing agents simultaneously, it is characterized in that comprising the following steps:
1) preparation of hybrid standard working solution: take 5 kinds of isothiazoline class antibacterial finishing agent standard items respectively, by 5 kinds of isothiazoline class antibacterial finishing agent standard items mixing, potpourri methyl alcohol is configured to the Standard Stock solutions that concentration is 1000mg/L, pipette the hybrid standard stock solution of 5 kinds of isothiazolinone antibacterial finishing agents, be placed in brown volumetric flask, be settled to scale with methanol dilution, shake up;
2) liquid phase chromatogram condition:
Chromatographic column is XR-ODS, and internal diameter is 100mm × 3.0mm, and column temperature is 40 DEG C, and column flow rate is 0.4mL/min, and adopt diode array detector, determined wavelength is respectively 277nm and 283nm, and when condition of gradient elution is initial, the volume ratio of methyl alcohol and water is 40:60; The volume ratio 90:10 that 1.90min internal linear changes methyl alcohol and water into keeps 6.00min; Change the volume ratio 40:60 of methyl alcohol and water during 6.01min into, keep 9.00min;
3) measure
By step 1) the hybrid standard working solution 1uL for preparing injects high performance liquid chromatograph, in step 2) carry out gradient elution under the liquid phase chromatogram condition that sets.
10. detection method as claimed in claim 9, it is characterized in that described 5 kinds of isothiazolinone antibacterial finishing agents are MIT, the chloro-2 methyl-4-isothiazoline-3-ketone of 5-, 1,2-benzisothiazole-3-ketone, Kathon, 4,5-bis-chloro-Kathons.
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| CN105842351A (en) * | 2016-03-17 | 2016-08-10 | 贵州中烟工业有限责任公司 | Method for rapid determination of isothiazolinone compounds in water-based adhesive for cigarettes |
| CN106770851A (en) * | 2016-12-21 | 2017-05-31 | 广东省农业科学院农业生物基因研究中心 | A kind of mobile phase formula of liquid chromatography for measuring carotenoid and its application |
| CN107543878A (en) * | 2017-08-08 | 2018-01-05 | 浙江中烟工业有限责任公司 | A kind of method that 3 kinds of OIT preservatives in cigarette paper are determined using Liquid Chromatography-Tandem Mass Spectrometry |
| CN107589202A (en) * | 2017-09-22 | 2018-01-16 | 广州中科检测技术服务有限公司 | A kind of detection method of two kinds of preservatives in measure airstrainer |
| CN108169371A (en) * | 2017-12-21 | 2018-06-15 | 上海微谱化工技术服务有限公司 | The method for quantitatively determining of fungicide in a kind of coating |
| CN108548744A (en) * | 2018-02-10 | 2018-09-18 | 安徽省产品质量监督检验研究院（国家排灌及节水设备产品质量监督检验中心） | In a kind of wet tissue the simulation of isothiazolinone preservative using the rate of transform assay method |
| CN110068620A (en) * | 2018-01-23 | 2019-07-30 | 苏州电器科学研究院股份有限公司 | A kind of method of isothiazolinone biocide agent content in quick detection textile |
| CN115343393A (en) * | 2022-08-23 | 2022-11-15 | 福建省纤维检验中心 | Method for detecting 1-vinyl imidazole in fabric |
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| CN105842351A (en) * | 2016-03-17 | 2016-08-10 | 贵州中烟工业有限责任公司 | Method for rapid determination of isothiazolinone compounds in water-based adhesive for cigarettes |
| CN105842351B (en) * | 2016-03-17 | 2020-11-20 | 贵州中烟工业有限责任公司 | Method for rapidly detecting isothiazolinone compounds in water-based adhesive for cigarettes |
| CN106770851A (en) * | 2016-12-21 | 2017-05-31 | 广东省农业科学院农业生物基因研究中心 | A kind of mobile phase formula of liquid chromatography for measuring carotenoid and its application |
| CN107543878A (en) * | 2017-08-08 | 2018-01-05 | 浙江中烟工业有限责任公司 | A kind of method that 3 kinds of OIT preservatives in cigarette paper are determined using Liquid Chromatography-Tandem Mass Spectrometry |
| CN107589202A (en) * | 2017-09-22 | 2018-01-16 | 广州中科检测技术服务有限公司 | A kind of detection method of two kinds of preservatives in measure airstrainer |
| CN107589202B (en) * | 2017-09-22 | 2020-05-15 | 广州中科检测技术服务有限公司 | Detection method for determining two preservatives in air filter screen |
| CN108169371A (en) * | 2017-12-21 | 2018-06-15 | 上海微谱化工技术服务有限公司 | The method for quantitatively determining of fungicide in a kind of coating |
| CN110068620A (en) * | 2018-01-23 | 2019-07-30 | 苏州电器科学研究院股份有限公司 | A kind of method of isothiazolinone biocide agent content in quick detection textile |
| CN108548744A (en) * | 2018-02-10 | 2018-09-18 | 安徽省产品质量监督检验研究院（国家排灌及节水设备产品质量监督检验中心） | In a kind of wet tissue the simulation of isothiazolinone preservative using the rate of transform assay method |
| CN115343393A (en) * | 2022-08-23 | 2022-11-15 | 福建省纤维检验中心 | Method for detecting 1-vinyl imidazole in fabric |
| CN115343393B (en) * | 2022-08-23 | 2023-09-26 | 福建省纤维检验中心 | Method for detecting 1-vinyl imidazole in fabric |
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