CN103048319B - Method for detecting residual disinfecting Cetyltrimethylammonium Chloride used in production process of sodium hyaluronate - Google Patents
Method for detecting residual disinfecting Cetyltrimethylammonium Chloride used in production process of sodium hyaluronate Download PDFInfo
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Abstract
The invention relates to a method for detecting residual disinfecting Cetyltrimethylammonium Chloride (CTAC) used in the production process of sodium hyaluronate. The method comprises the following steps: preparing a CTAC standard solution to structure a linear regression equation; preparing a sample solution, using an improved bismuth potassium iodide test solution for developing and measuring the absorbency value; and calculating the content of the CTAC with the linear regression equation. The structuring method of the linear regression equation is as follows: after using the improved bismuth potassium iodide test solution for developing of the prepared 2 Mug/ml, 4 Mug/ml, 8 Mug/ml, 10 Mug/ml and 20 Mug/ml standard solutions, measuring the absorbency under 290nm. By adopting the method to detect the content of the CTAC, the shortcoming that the content and the residue of the CTAC serving as a disinfectant or a reaction agent can not be monitored at present can be overcome, the detection time is greatly shortened, and the detection cost is lowered. The method provided by the invention is particularly suitable for detecting CTAC in labs.
Description
Technical field:
The present invention relates to a kind of detection method of hexadecyltrimethylammonium chloride, is espespecially the detection method of the hexadecyltrimethylammonium chloride that in production run, cleaning-sterilizing remains.
Background technology:
The Chinese another name of hexadecyltrimethylammonium chloride: cetane trimethyl ammonium chloride; CTAC; 1631, chlorination trimethylcetylammonium.
English name: Hexadecyl trimethylammonium chloride, structural formula is as follows:
English another name: CTAC; Cetyltrimethylammonium chloride
No. CAS: 112-02-7
Molecular formula: C19H42ClN
Linear formula: CH3 (CH2) 15N (Cl) (CH3) 3
Molecular weight: 320.00
Purity: >=99%
No. MDL: MFCD00011773
No. Beilstein: 3657974
No. EC: 203-928-6
Hexadecyltrimethylammonium chloride is white crystalline powder, is soluble in isopropyl alcohol, water soluble, produces a large amount of foam during concussion, can have good compatibility with kation, nonionic, amphoteric surfactant; Chemical stability is good, heat-resisting, fast light, withstand voltage, strong alkali-acid resistance; There is excellent infiltration, softening, emulsification, antistatic, the performance such as biodegradability and sterilization.Be widely used in medical industry auxiliary agent, protein flocculation and water treatment flocculation, sanitizer, cleaning and disinfecting sterilization etc.
Hexadecyltrimethylammonium chloride MSDS data is shown as toxicity 4 grades, moderate toxicity, and LD50 is 400mg/kg.Therefore consider in view of the safety in utilization of product, be necessary to carry out the detection of residual quantity limit to CTAC residual in product.In document disclosed at present, no matter be American Pharmacopeia or Japanese Pharmacopoeia, there is no the detection method for this content of material or residual volume at present.
Summary of the invention:
The object of this invention is to provide the detection method of the residual hexadecyltrimethylammonium chloride of sterilization in a kind of sodium hyaluronate production run, caused safety issue is remained to solve hexadecyltrimethylammonium chloride, the method detects accurately, and inspection cost, checkability are high, inspection work is carried out conveniently.
For realizing object of the present invention, the technical solution adopted in the present invention is:
A detection method for the residual hexadecyltrimethylammonium chloride of sterilization in sodium hyaluronate production run, is characterized in that, comprise the following steps:
(1) preparation of typical curve: take hexadecyltrimethylammonium chloride reference substance, adds hydrochloric acid solution and the constant volume that is dissolved in water, is mixed with hexadecyltrimethylammonium chloride storing solution; Hexadecyltrimethylammonium chloride storing solution is diluted, is mixed with the hexadecyltrimethylammonium chloride titer of 2 μ g/ml, 4 μ g/ml, 8 μ g/ml, 10 μ g/ml, 20 μ g/ml; Pipette each hexadecyltrimethylammonium chloride titer of certain volume, be placed in test tube, the isopyknic described hydrochloric acid solution of titer is pipetted in two blank tubes, improvement bismuth potassium iodide test solution is added in above-mentioned each pipe, immediately in the mixing of vortex oscillator, room temperature places 5-15min, take blank tube as contrast, survey the absorbance under 290nm, draw linear regression equation;
(2) sample solution preparation: take/pipette hexadecyltrimethylammonium chloride sample, be dissolved in water after adding described hydrochloric acid solution constant volume, adds improvement bismuth potassium iodide test solution, mix at vortex oscillator immediately, room temperature places 5-15min, take blank tube as contrast, surveys the absorbance under 290nm; Described hexadecyltrimethylammonium chloride sample is after using hexadecyltrimethylammonium chloride sterilization, the Liquid Residue that may contain hexadecyltrimethylammonium chloride after cleaning up by purified water;
(3) by linear regression equation, the content of hexadecyltrimethylammonium chloride is calculated.
In a preferred embodiment of the invention, the concentration of described hydrochloric acid solution is 0.6mol/L; Wherein in step (1) and step (2), the amount adding hydrochloric acid solution is 2ml.
In a preferred embodiment of the invention, in step (1) and step (2), the amount adding improvement bismuth potassium iodide test solution is 0.5ml.
The preparation method of described improvement bismuth potassium iodide test solution gets basic bismuth nitrate 0.85g, adds after glacial acetic acid 10ml and water 40ml dissolves, adds liquor kalii iodide (4 → 10) 20ml, shake up to obtain test solution, then pipette above-mentioned test solution 1ml, add 0.6mol/L hydrochloric acid solution 2ml, add water to 10ml, to obtain final product.
In a preferred embodiment of invention, in step (2), the amount taking/pipette hexadecyltrimethylammonium chloride sample is 10mg.
The Cleaning Principle of the detection method of hexadecyltrimethylammonium chloride of the present invention reacts according to the amino contained in hexadecyltrimethylammonium chloride molecule and improvement bismuth potassium iodide test solution, produce violet compound, this compound can produce absorption maximum at 290nm place.
Method of the present invention is utilized to detect hexadecyltrimethylammonium chloride content, make up current hexadecyltrimethylammonium chloride as the shortcoming cannot monitoring its content and residual volume when sanitizer or reaction reagent, substantially reduce detection time, reduce testing cost, be particularly suitable for the detection that the right hexadecyltrimethylammonium chloride content in laboratory carries out.
Embodiment
Can be well understood to the present invention further by specific embodiments of the invention given below, but they not limitation of the invention.
Embodiment
(1) take hexadecyltrimethylammonium chloride reference substance, add 0.6mol/L hydrochloric acid solution 2ml, be dissolved in water constant volume, is mixed with the hexadecyltrimethylammonium chloride storing solution of 200 μ g/ml; Hexadecyltrimethylammonium chloride storing solution is diluted, is mixed with the titer of 1 μ g/ml, 2 μ g/ml, 4 μ g/ml, 8 μ g/ml, 10 μ g/ml; Pipette each titer of certain volume, be placed in test tube, the isopyknic 0.6mol/L hydrochloric acid solution of titer is pipetted in two blank tubes, improvement bismuth potassium iodide test solution 0.5ml is added in above-mentioned each pipe, immediately in the mixing of vortex oscillator, room temperature places 5-15min, take blank tube as contrast, survey the absorbance under 290nm, draw linear regression equation;
(2) sample solution preparation: take/pipette hexadecyltrimethylammonium chloride sample 5ml, add 0.6mol/L hydrochloric acid solution 2ml, be dissolved in water and be settled to 10ml, add improvement bismuth potassium iodide test solution 0.5ml, mix at vortex oscillator immediately, room temperature places 5-15min, take blank tube as contrast, surveys the absorbance under 290nm; Hexadecyltrimethylammonium chloride sample is after using hexadecyltrimethylammonium chloride sterilization, the Liquid Residue that may contain hexadecyltrimethylammonium chloride after cleaning up by purified water.
(3) by linear regression equation, the content of hexadecyltrimethylammonium chloride is calculated.
Improvement bismuth potassium iodide test solution gets basic bismuth nitrate 0.85g, adds after glacial acetic acid 10ml and water 40ml dissolves, add liquor kalii iodide (4 → 10) 20ml, shake up, then pipette above-mentioned test solution 1ml, add 0.6mol/L hydrochloric acid solution 2ml, add water to 10ml, to obtain final product.
Test findings:
After using hexadecyltrimethylammonium chloride sterilization according to the method for above-described embodiment to three times, the three place's Liquid Residue content detection that may contain hexadecyltrimethylammonium chloride after cleaning up by purified water the results are shown in Table 1:
Table 1
As known from Table 1, after method of the present invention uses hexadecyltrimethylammonium chloride sterilization to three times, may test by three place's Liquid Residues containing hexadecyltrimethylammonium chloride after cleaning up by purified water, compensate for the blank not having the method at present, improves detection efficiency, accelerate sample dissolution, sample is easy to mixing, avoids the metrical error because incomplete mixing brings, and reduces the use amount of reagent, reduce inspection cost, ensure that the safety of medicine.
Claims (5)
1. in sodium hyaluronate production run, sterilization remains a detection method for hexadecyltrimethylammonium chloride, it is characterized in that, comprises the following steps:
(1) preparation of typical curve: take hexadecyltrimethylammonium chloride reference substance, adds hydrochloric acid solution and the constant volume that is dissolved in water, is mixed with hexadecyltrimethylammonium chloride storing solution; Hexadecyltrimethylammonium chloride storing solution is diluted, is mixed with the hexadecyltrimethylammonium chloride titer of 1 μ g/ml, 2 μ g/ml, 4 μ g/ml, 8 μ g/ml, 10 μ g/ml; Pipette each hexadecyltrimethylammonium chloride titer of certain volume, be placed in test tube, the isopyknic described hydrochloric acid solution of titer is pipetted in two blank tubes, improvement bismuth potassium iodide test solution is added in above-mentioned each pipe, immediately in the mixing of vortex oscillator, room temperature places 5-15min, take blank tube as contrast, survey the absorbance under 290nm, draw linear regression equation;
(2) sample solution preparation: take/pipette hexadecyltrimethylammonium chloride sample, be dissolved in water after adding described hydrochloric acid solution constant volume, adds improvement bismuth potassium iodide test solution, mix at vortex oscillator immediately, room temperature places 5-15min, take blank tube as contrast, surveys the absorbance under 290nm; Described hexadecyltrimethylammonium chloride sample is after using hexadecyltrimethylammonium chloride sterilization, the Liquid Residue that may contain hexadecyltrimethylammonium chloride after cleaning up by purified water;
(3) by linear regression equation, the content of hexadecyltrimethylammonium chloride is calculated.
2. the detection method of hexadecyltrimethylammonium chloride as claimed in claim 1, it is characterized in that, the concentration of described hydrochloric acid solution is 0.6mol/L; Wherein in step (1) and step (2), the amount adding hydrochloric acid solution is 2ml.
3. the detection method of the residual hexadecyltrimethylammonium chloride of sterilization in a kind of sodium hyaluronate production run as claimed in claim 1, is characterized in that, in step (1) and step (2), adding the amount improveing bismuth potassium iodide test solution is 0.5ml.
4. in a kind of sodium hyaluronate production run as claimed in claim 1, sterilization remains the detection method of hexadecyltrimethylammonium chloride, it is characterized in that, the preparation method of described improvement bismuth potassium iodide test solution gets basic bismuth nitrate 0.85g, add after glacial acetic acid 10ml and water 40ml dissolves, add liquor kalii iodide (4 → 10) 20ml, shake up to obtain test solution, pipette above-mentioned test solution 1ml again, add 0.6mol/L hydrochloric acid solution 2ml, add water to 10ml, to obtain final product.
5. in a kind of sodium hyaluronate production run as claimed in claim 1, sterilization remains the detection method of hexadecyltrimethylammonium chloride, and it is characterized in that, in step (2), the amount taking/pipette hexadecyltrimethylammonium chloride sample is 10mg.
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| CN103389300A (en) * | 2013-08-13 | 2013-11-13 | 南京大学 | Method for detecting quaternary ammonium salt cationic surfactant |
| CN103616379B (en) * | 2013-12-04 | 2015-09-09 | 江苏天诺新材料科技股份有限公司 | The quantitative determination method of 4-propyl bromide content in zeolite synthesis waste liquid |
| CN104237219B (en) * | 2014-08-20 | 2016-08-24 | 浙江大学 | A kind of water quality quaternary ammonium salt semi-quantitative detection method |
| CN106442841B (en) * | 2016-12-16 | 2018-09-14 | 上海景峰制药有限公司 | The method for separating and detecting of cationic surfactant in a kind of drug |
| CN112773734A (en) * | 2020-12-28 | 2021-05-11 | 杭州欧菲健康科技有限公司 | Hyaluronic acid skin-changing essence and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1292089A (en) * | 1998-01-28 | 2001-04-18 | 克拉里安特国际有限公司 | Determining method for concentration of nonionic surfactants is aqueous alkaline solutions |
| CN101852739A (en) * | 2010-05-21 | 2010-10-06 | 东北师范大学 | Method for determining polysorbate nonionic surfactant |
-
2012
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1292089A (en) * | 1998-01-28 | 2001-04-18 | 克拉里安特国际有限公司 | Determining method for concentration of nonionic surfactants is aqueous alkaline solutions |
| CN101852739A (en) * | 2010-05-21 | 2010-10-06 | 东北师范大学 | Method for determining polysorbate nonionic surfactant |
Non-Patent Citations (4)
| Title |
|---|
| Fluorescence-detecting cationic surfactants using luminescent CdTe quantum dots as probes;Xue-Lian Diao et al.;《Analytical and Bioanalytical Chemistry》;20071231;第388卷(第5-6期);1191-1197 * |
| Tensammetric studies of the separation of surfactants Part 1.Investigation of sources of error in precipitation of non-ionic surfactants with modified Dragendorff reagent;Bogdan Wyrwas et al.;《Analytica Chimica Acta》;19931221;第278卷(第1期);197-203 * |
| 双十八烷基二甲基氯化铵活性物含量的紫外-可见光度法测定;陈鑫琪 等;《工业水处理》;20120229;第32卷(第2期);77-79 * |
| 溴甲酚紫-十六烷基二甲基苄基溴化铵法测定废水中阴离子表面活性剂含量;李来丙 等;《化工环保》;20051231;第25卷(第1期);68-71 * |
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Address after: 200120 Shanghai city Baoshan District Luo Road No. 50 Patentee after: Shanghai Jingfeng Pharmaceutical Co., Ltd. Address before: 200120 Shanghai city Baoshan District Luo Road No. 50 Patentee before: Shanghai Jingfeng Pharmaceutical Co., Ltd. |