CN106198774A - The method of impurity, the method for preparation ZUGUANG SAN and ZUGUANG SAN in detection salicylic acid sample - Google Patents
The method of impurity, the method for preparation ZUGUANG SAN and ZUGUANG SAN in detection salicylic acid sample Download PDFInfo
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- CN106198774A CN106198774A CN201610463426.XA CN201610463426A CN106198774A CN 106198774 A CN106198774 A CN 106198774A CN 201610463426 A CN201610463426 A CN 201610463426A CN 106198774 A CN106198774 A CN 106198774A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention provides the method for impurity in detection salicylic acid sample, the method for preparation ZUGUANG SAN and ZUGUANG SAN.Wherein, in detection salicylic acid sample, the method for impurity includes: utilize high performance liquid chromatography to contain described salicylic acid sample detection, the flowing of wherein said high performance liquid chromatography mutually: 40 59 parts by volume methanol；41 60 parts by volume water；And 0.2 1 parts by volume glacial acetic acid.Use this detection method, it is possible to the impurity content in detection salicylic acid sample effectively.
Description
Technical field
The present invention relates to field of medicaments.In particular it relates to detect the method for impurity in salicylic acid sample, preparation foot
The method that light dissipates and the ZUGUANG SAN utilizing the method to prepare.
Background technology
At present, ZUGUANG SAN is mainly used in the treatment of Keratotic tinea hand or pedis and fetid sweat.
ZUGUANG SAN be mainly composed of salicylic acid, benzoic acid, boric acid, Radix Sophorae Flavescentis.The quality of the raw materials such as salicylic acid such as impurity
Content, by preparation efficiency and the yield rate of appreciable impact ZUGUANG SAN.But, at present for former during producing ZUGUANG SAN
The detection means of material still haves much room for improvement.
Summary of the invention
It is contemplated that one of technical problem solved the most to a certain extent in correlation technique.
The present invention is following discovery based on inventor and completes:
The present inventor finds in research process, salicylic acid high performance liquid chromatography described in " Chinese Pharmacopoeia "
There is at least one its own shortcomings in detection method: Detection results is poor, the separating degree of impurity peaks does not meets States Pharmacopoeia specifications, this pharmacopeia rule
Fixed method all cannot realize examination criteria for multiple chromatographic column, thus have impact on the preparation efficiency of ZUGUANG SAN, production cost
Higher.Inventor finds through further investigation, in the flowing phase composition meeting appreciable impact salicylic acid sample of high performance liquid chromatography
The Detection results of impurity.
In view of this, it is an object of the present invention to propose one can effectively impurity in salicylic acid sample be examined
The method surveyed.
In a first aspect of the present invention, the present invention proposes and a kind of detects the method for impurity in salicylic acid sample.According to this
Inventive embodiment, impurity include selected from 4-HBA, 4 hydroxyisophthalic acid and phenol at least one, and should
Method includes: utilizing high performance liquid chromatography to described sample detection, wherein, the flowing of described high performance liquid chromatography contains mutually
Have: 40-59 parts by volume methanol；41-60 parts by volume water；And 0.2-1 parts by volume glacial acetic acid.
Inventor is it was unexpectedly observed that use detection method according to embodiments of the present invention, by using the phase that specifically flows
Composition can detect the impurity in salicylic acid sample effectively, improves the separating effect of Detection results and impurity peaks, thus
Improve further and salicylic acid raw material is used for preparing the efficiency of ZUGUANG SAN.
It addition, the method for impurity can also have the most attached in detection salicylic acid sample according to the above embodiment of the present invention
The technical characteristic added:
According to embodiments of the invention, described flowing contains mutually: 45-59 parts by volume methanol；41-55 parts by volume water；And
0.3-0.5 parts by volume glacial acetic acid.Thus, it is possible to the most more effectively detect the impurity in salicylic acid sample, improve detection sample
The effect of salicylic method in product, thus improve the efficiency that salicylic acid raw material is used for preparing ZUGUANG SAN further.
According to embodiments of the invention, described flowing contains mutually: 50 parts by volume methanol；50 parts by volume water；And 1 parts by volume
Glacial acetic acid.Thus, it is possible to the most more effectively detect the impurity in salicylic acid sample, improve salicylic side in detection sample
The effect of method, thus improve the efficiency that salicylic acid raw material is used for preparing ZUGUANG SAN further.
According to embodiments of the invention, described flowing contains mutually: 40 parts by volume methanol；60 parts by volume water；And 0.3 volume
Part glacial acetic acid.Thus, it is possible to the most more effectively detect the impurity in salicylic acid sample, improve in detection sample salicylic
The effect of method, thus improve the efficiency that salicylic acid raw material is used for preparing ZUGUANG SAN further.
According to embodiments of the invention, described flowing contains mutually: 45 parts by volume methanol；55 parts by volume water；And 0.5 volume
Part glacial acetic acid.Thus, it is possible to the most more effectively detect the impurity in salicylic acid sample, improve in detection sample salicylic
The effect of method, thus improve the efficiency that salicylic acid raw material is used for preparing ZUGUANG SAN further.
According to embodiments of the invention, the described high performance liquid chromatography following condition of employing: chromatographic column: use C18 chromatograph
Post, preferably Agilient Eclipse XDB-C18 4.6*150mm 5 microns, 5 microns of 4.6mm* of Yi Lite Sinopak C18
At least one 150mm and ohm Buddhist nun 5 microns of 4.6mm*150mm of Hubble C18；Column temperature: 30 degrees Celsius；Flow velocity: 1.0mL/
min；Or sample size: 20 microlitres.Thus, it is possible to the most more effectively detect the impurity in salicylic acid sample, improve detection sample
The effect of salicylic method in product, thus improve the efficiency that salicylic acid raw material is used for preparing ZUGUANG SAN further.It addition, this
The inventor of invention is it was unexpectedly observed that the method for impurity in detection salicylic acid sample according to embodiments of the present invention, it is possible to effectively
Ground is applicable to multiple conventional chromatographic column；And for the method for impurity in detection salicylic acid corresponding in pharmacopeia, inventor is many
Plant and tested in conventional chromatographic column, be all not carried out preferable Detection results.
In a second aspect of the present invention, the present invention proposes and a kind of detects the method for impurity in salicylic acid sample, its feature
It is, including: use high performance liquid chromatograph model: Yi Lite 1201 that salicylic acid sample is detected, wherein,
Chromatographic condition: chromatographic column be Agilient Eclipse XDB-C18 and specification be 4.6*150mm, packing material size be
5 microns, detecting wavelength 270nm, column temperature is 30 degrees Celsius, and flow velocity is 1.0mL/min, and sample size is 20 microlitres, and flowing is first mutually
Alcohol-water-glacial acetic acid (volume ratio is 45:55:0.5)；
In described detection, weigh salicylic acid product 0.5g, be placed in 100mL measuring bottle, add flowing phased soln and be diluted to,
As need testing solution；
From obtained need testing solution, take 1mL, be placed in 50mL measuring bottle, with flowing phase dilution, shake up, more accurate amount
Take 1mL, be placed in 10mL measuring bottle, then with flowing phase dilution extremely, concentration is every milliliter of microgram Han salicylic acid 10, shakes up, as right
According to solution；
Take the 4-HBA of scheduled volume, 4 hydroxyisophthalic acid and phenol reference substance, add flowing phased soln dilute
Release and make mixed solution as reference substance solution, wherein containing 4-HBA 5 microgram, 4-hydroxyl in every this mixed solution of 1mL
Base M-phthalic acid 2.5 microgram and phenol 1 microgram.
Inventor is it was unexpectedly observed that use the detection method of the embodiment of the present invention, it is possible to detection salicylic acid sample effectively
In impurity, improve the separating effect of Detection results and impurity peaks, thus improve further and be used for preparing by salicylic acid raw material
The efficiency of ZUGUANG SAN.
In a third aspect of the present invention, the present invention proposes a kind of method preparing ZUGUANG SAN.Enforcement according to the present invention
Example, the method includes: (a) method as described above, detects the impurity in candidate's salicylic acid raw material；(b) based on
Testing result obtained by step (a), selects acceptable material from described candidate feed；And (c) utilizes described qualified former
Described ZUGUANG SAN prepared by material.As it was previously stated, inventor is it was unexpectedly observed that use preparation method according to embodiments of the present invention, energy
Enough it is effectively improved the efficiency of preparation ZUGUANG SAN, improves the production yields of ZUGUANG SAN, or reduce the production cost of ZUGUANG SAN.This
Skilled person is it is understood that above for feature and advantage described by salicylic method in detection sample, still
It is applicable to this method preparing ZUGUANG SAN, does not repeats them here.
In addition, it is necessary to explanation, those skilled in the art can select the salicylic acid that impurity content is relatively low as required
Sample is prepared ZUGUANG SAN.According to one embodiment of present invention, it is preferred to use meet the salicylic acid sample of one of following standard
Product, as acceptable material, more preferably meet employing and meet the salicylic acid sample of following standard as acceptable material:
The content of 4-HBA is less than 0.1 weight %；
Between 4-hydroxyl, the content of dibenzoic acid is less than 0.05 weight %；And
The content of phenol is less than 0.02 weight %.
Those skilled in the art, can be determined based on high performance liquid chromatography testing result by any of method
The content of impurity in salicylic acid sample, such as can be by right with impurity institute in external standard method spectrogram based on high performance liquid chromatography
The area of Ying Feng determines the content of corresponding impurity.It addition, according to the concrete example of the present invention, acceptable material meets following further
Standard:
The area of other single impurity peaks is not more than 0.25 times of the main peak area of contrast solution, and (content of conversion is 0.05
Weight %), each impurity peak area and no more than contrast solution main peak area (content of conversion is 0.2 weight %).
In a fourth aspect of the present invention, the present invention proposes a kind of ZUGUANG SAN, according to embodiments of the invention, described sufficient light
Scattered is to be prepared by the method for foregoing preparation ZUGUANG SAN.As it was previously stated, use the preparation method of the embodiment of the present invention,
The efficiency of preparation ZUGUANG SAN can be effectively improved, improve the production yields of ZUGUANG SAN, or reduce the production cost of ZUGUANG SAN.
Thus this ZUGUANG SAN has, and production efficiency is high, yields is high or low cost and other advantages.Skilled artisans appreciate that
It is, above for the feature and advantage described by the method for salicylic method and preparation ZUGUANG SAN in detection sample, still to fit
The method preparing ZUGUANG SAN for this, does not repeats them here.
The additional aspect of the present invention and advantage will part be given in the following description, and part will become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or the additional aspect of the present invention and advantage are from combining the accompanying drawings below description to embodiment and will become
Substantially with easy to understand, wherein:
Fig. 1 is the chromatogram of reference substance solution according to an embodiment of the invention；
Fig. 2 is the chromatogram of reference substance solution in accordance with another embodiment of the present invention；
Fig. 3 is the chromatogram of reference substance solution in accordance with another embodiment of the present invention；
Fig. 4 is the chromatogram of contrast solution in accordance with another embodiment of the present invention；
Fig. 5 is the chromatogram of need testing solution in accordance with another embodiment of the present invention；
Fig. 6 is the chromatogram of reference substance solution in accordance with another embodiment of the present invention；
Fig. 7 is the chromatogram of reference substance solution in accordance with another embodiment of the present invention；
Fig. 8 is the chromatogram of reference substance solution in accordance with another embodiment of the present invention.
Detailed description of the invention
Embodiments of the invention are described below in detail, and those skilled in the art is it will be appreciated that example below is intended to for solving
Release the present invention, and be not construed as limitation of the present invention.Unless stated otherwise, embodiment below is not expressly recited specifically
Technology or condition person, those skilled in the art can be according to the conventional technology in this area or condition or according to the description of product
Book is carried out.Agents useful for same or instrument unreceipted production firm person, be can by city available from conventional products.
Conventional method
Unless expressly stated, following instrument and testing conditions is used to carry out chromatography in the examples below that:
High performance liquid chromatograph model: Yi Lite 1201.
Chromatographic condition: chromatographic column be Agilient Eclipse XDB-C18 and specification be 4.6*150mm, packing material size be
5 microns, detecting wavelength 270nm, column temperature is 30 degrees Celsius, and flow velocity is 1.0mL/min, and sample size is 20 microlitres, and flowing contains mutually
The mixture (volume ratio specifically limits in embodiment below and comparative example) of methanol, water and glacial acetic acid.
Reagent: 4-HBA reference substance (purchased from National Institute for Food and Drugs Control), 4 hydroxyisophthalic acid
Reference substance (purchased from National Institute for Food and Drugs Control), phenol reference substance (purchased from National Institute for Food and Drugs Control), first
Alcohol (purchased from Tianjin Ke Miou chemical reagent company limited) and glacial acetic acid (purchased from Tianjin great Mao chemical reagent factory).
Preparation need testing solution: weigh salicylic acid product 0.5g, be placed in 100mL measuring bottle, adds flowing phased soln and dilutes
To every milliliter containing salicylic acid 5 milligrams, as need testing solution.
Configuration contrast solution: from obtained need testing solution, take 1mL, be placed in 50mL measuring bottle, with flowing phase dilution,
Shake up, then precision measure 1mL, be placed in 10mL measuring bottle, then with flowing phase dilution to every milliliter of microgram Han salicylic acid 10, shake up,
As contrast solution.
Configuration reference substance solution: take the 4-HBA of scheduled volume, 4 hydroxyisophthalic acid and phenol reference substance, add
Flowing phased soln also dilutes and makes mixed solution as reference substance solution, wherein contains 4-hydroxy benzenes in every this mixed solution of 1mL
Formic acid 5 microgram, 4 hydroxyisophthalic acid 2.5 microgram and phenol 1 microgram.
Embodiment 1
In this embodiment, according to the method essentially identical with conventional method and condition, take reference substance solution 20 microlitre note
Enter high performance liquid chromatograph, reference substance solution is detected.Difference is, the flowing used in this embodiment is mutually for first
Alcohol-water-glacial acetic acid (volume ratio is 50:50:1).
As it is shown in figure 1, wherein, No. 1 peak represents 4-HBA to chromatogram obtained by this embodiment, and No. 2 peaks represent
4 hydroxyisophthalic acid, No. 3 peaks represent phenol.As seen from Figure 1, No. 1 peak returns to baseline position, and with No. 2 peaks point
Reaching 3.00 from degree, No. 2 peaks and No. 3 peaks return to substantially baseline, and separating degree is 1.62, meet chromatogram in " Chinese Pharmacopoeia " each
The requirement more than 1.5 of the peak separating degree.
Embodiment 2
In this embodiment, according to method substantially the same manner as Example 1, reference substance solution is detected.Distinguish
In, the flowing used in this embodiment is mutually for methanol-water-glacial acetic acid (volume ratio is 40:60:0.3).
Chromatogram obtained by this embodiment is as shown in Figure 2.As seen from Figure 2,3 impurity peaks are returned to baseline position
Put, and the separating degree between No. 1 peak and No. 2 peaks is 2.25, and the separating degree between No. 2 peaks and No. 3 peaks reaches 3.80.Impurity peaks
Separating effect comply fully with the separating degree requirement in " Chinese Pharmacopoeia ".
Embodiment 3
In this embodiment, according to method substantially the same manner as Example 2, reference substance solution is detected.Distinguish
In, the flowing used in this embodiment is mutually for methanol-water-glacial acetic acid (volume ratio is 45:55:0.5).
Chromatogram obtained by this embodiment is as shown in Figure 3.As seen from Figure 3,3 impurity peaks are returned to baseline position
Put, and the separating degree between No. 1 peak and No. 2 peaks is 4.05, and the separating degree between No. 2 peaks and No. 3 peaks reaches 3.04.Impurity peaks
Separating effect comply fully with the separating degree requirement in " Chinese Pharmacopoeia ".
Can obtain from Fig. 3,3 respective retention times of impurity peaks and peak area, not repeat them here.
Embodiment 4
In this embodiment, according to method substantially the same manner as Example 3, salicylic acid sample solution is detected.Should
The flowing used in embodiment is mutually for methanol-water-glacial acetic acid (volume ratio is 45:55:0.5).
As shown in Figure 4, the chromatogram of need testing solution is as shown in Figure 5 for the chromatogram of the contrast solution of this embodiment.
Can obtain from Fig. 4 of contrast solution, retention time be the salicylic peak area of 6.318min be 52.55mV
sec.For other impurity beyond 4-HBA, 4 hydroxyisophthalic acid or phenol, each impurity peak area must not
More than 0.25 times (content of conversion is 0.05 weight %) of this main peak area, and each impurity peak area sum is not more than this main peak
Area (content of conversion is 0.2 weight %).
Can be seen that from Fig. 5 of need testing solution, use the mobile phase ratio of this embodiment can efficiently separate three miscellaneous
Mass peak.And, converted by the ratio of each impurity peak area impurity peak area corresponding with Fig. 3, can obtain: 0.5 gram
In salicylic acid product, the content of 4-HBA impurity is 4.30 micrograms, and the content of 4 hydroxyisophthalic acid impurity is
0.94 microgram, the content of Phenol contamination is 0.33 microgram, meets the regulation of " Chinese Pharmacopoeia ".So, it can be determined that this salicylic acid
Product can be as acceptable material, for the production and application of ZUGUANG SAN.
Embodiment 5
In this embodiment, according to method substantially the same manner as Example 3, reference substance solution is detected.Distinguish
In, use following chromatographic column:
5 microns of 4.6mm*150mm of Yi Lite Sinopak C18；
Ohm 5 microns of 4.6mm*150mm of Buddhist nun Hubble C18.
The chromatogram result that reference substance solution is detected by this embodiment by two kinds of chromatographic columns, respectively such as Fig. 6 and Fig. 7
Shown in.Use other two kinds of chromatographic columns as seen from the figure, can effectively detect the impurity in salicylic acid sample equally, change
Kind Detection results and the separating effect of impurity peaks.
Comparative example 1
In this comparative example, according to the method essentially identical with conventional method and condition, take reference substance solution 20 microlitre note
Enter high performance liquid chromatograph, reference substance solution is detected.Difference is, the flowing used in this comparative example is first mutually
Alcohol-water-glacial acetic acid (volume ratio is 60:40:1), i.e. listed with " Chinese Pharmacopoeia " method is essentially identical.
Chromatogram obtained by this embodiment is as shown in Figure 8.As seen from Figure 8,3 impurity peaks are all not returned to baseline
Separating degree between position, and 3 peaks is respectively 1.59 and 1.17, does not meets the separating degree requirement of " Chinese Pharmacopoeia ".
Comparative example 2
In this comparative example, according to the method essentially identical with comparative example 1 and condition, reference substance solution is detected.
Difference is, uses following chromatographic column in this comparative example:
5 microns of 4.6mm*150mm of Yi Lite Sinopak C18；
Ohm 5 microns of 4.6mm*150mm of Buddhist nun Hubble C18；
10 microns of 4.6mm*150mm of Yi Lite YWG C18.
Result shows, in chromatogram, the separating effect of impurity peaks does not all meet the separating degree requirement of " Chinese Pharmacopoeia ".
Sum up
Integrated embodiment 1～5 and comparative example 1～2 can draw, impurity in detection salicylic acid product proposed by the invention
Method can detect the impurity in salicylic acid sample effectively, improves Detection results and the separating effect of impurity peaks, thus enters one
Step improves and is used for preparing the efficiency of ZUGUANG SAN by salicylic acid raw material.It addition, according to embodiment 5 it can be seen that the method for the present invention
Multiple common chromatographic column can be applicable to.
By comparative example 1 with 2 it can be seen that be methanol-water-glacial acetic acid (volume ratio is 60:40:1) mutually for flowing
Situation, inventor has attempted multiple chromatographic column, does not all meet the separating degree requirement of " Chinese Pharmacopoeia ", thus, it is possible to find out flowing
The proportion of composing of phase is to affect the key factor of defects inspecting efficiency in salicylic acid sample.
In the description of this specification, reference term " embodiment ", " some embodiments ", " example ", " specifically show
Example " or the description of " some examples " etc. means to combine this embodiment or example describes specific features, structure, material or spy
Point is contained at least one embodiment or the example of the present invention.In this manual, to the schematic representation of above-mentioned term not
Identical embodiment or example must be directed to.And, the specific features of description, structure, material or feature can be in office
One or more embodiments or example combine in an appropriate manner.Additionally, in the case of the most conflicting, the skill of this area
The feature of the different embodiments described in this specification or example and different embodiment or example can be tied by art personnel
Close and combination.
Although above it has been shown and described that embodiments of the invention, it is to be understood that above-described embodiment is example
Property, it is impossible to being interpreted as limitation of the present invention, those of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, revises, replaces and modification.
Claims (9)
1. one kind is detected the method for impurity in salicylic acid sample, it is characterised in that described impurity include selected from 4-HBA,
At least one 4 hydroxyisophthalic acid and phenol, described method includes:
Utilizing high performance liquid chromatography to described salicylic acid sample detection, wherein, the flowing of described high performance liquid chromatography contains mutually
Have:
40-59 parts by volume methanol；
41-60 parts by volume water；And
0.2-1 parts by volume glacial acetic acid.
Method the most according to claim 1, it is characterised in that described flowing contains mutually:
45-59 parts by volume methanol；
41-55 parts by volume water；And
0.3-0.5 parts by volume glacial acetic acid.
Method the most according to claim 1, it is characterised in that described flowing contains mutually:
50 parts by volume methanol；
50 parts by volume water；And
1 parts by volume glacial acetic acid.
Method the most according to claim 1, it is characterised in that described flowing contains mutually:
40 parts by volume methanol；
60 parts by volume water；And
0.3 parts by volume glacial acetic acid.
Method the most according to claim 1, it is characterised in that described flowing contains mutually:
45 parts by volume methanol；
55 parts by volume water；And
0.5 parts by volume glacial acetic acid.
Method the most according to claim 1, it is characterised in that the described high performance liquid chromatography following condition of employing:
Chromatographic column: use C18 chromatographic column, preferably Agilient Eclipse XDB-C18 4.6*150mm 5 microns, Yi Lite
At least one 5 microns of 4.6mm*150mm of Sinopak C18 and ohm Buddhist nun 5 microns of 4.6mm*150mm of Hubble C18；
Column temperature: 30 degrees Celsius；
Flow velocity: 1.0mL/min；Or
Sample size: 20 microlitres.
7. one kind is detected the method for impurity in salicylic acid sample, it is characterised in that described impurity include selected from 4-HBA,
At least one 4 hydroxyisophthalic acid and phenol, described method includes:
Use high performance liquid chromatograph model: Yi Lite 1201 that salicylic acid sample is detected, wherein,
Chromatographic condition: chromatographic column be Agilient Eclipse XDB-C18 and specification be 4.6*150mm, packing material size be 5 micro-
Rice, detects wavelength 270nm, and column temperature is 30 degrees Celsius, and flow velocity is 1.0mL/min, and sample size is 20 microlitres, and flowing uses volume mutually
Than the methanol-water-glacial acetic acid for 45:55:0.5；
In described detection, weigh salicylic acid product 0.5g, be placed in 100mL measuring bottle, add flowing phased soln and be diluted to every milli
Rise containing salicylic acid 5 milligrams, as need testing solution；
From obtained need testing solution, take 1mL, be placed in 50mL measuring bottle, with flowing phase dilution, shake up, then precision measures
1mL, is placed in 10mL measuring bottle, then with flowing phase dilution to every milliliter of microgram Han salicylic acid 10, shakes up, as contrast solution；
Take the 4-HBA of scheduled volume, 4 hydroxyisophthalic acid and phenol reference substance, add flowing phased soln and dilute system
Become mixed solution as reference substance solution, wherein every this mixed solution of 1mL contains between 4-HBA 5 microgram, 4-hydroxyl
Phthalic acid 2.5 microgram and phenol 1 microgram.
8. the method preparing ZUGUANG SAN, it is characterised in that including:
A impurity in candidate's salicylic acid raw material, according to the method according to any one of claim 1～7, is detected by ()；
B (), based on testing result obtained in step (a), selects acceptable material from described candidate feed；And
C () utilizes described acceptable material to prepare described ZUGUANG SAN.
9. a ZUGUANG SAN, it is characterised in that described ZUGUANG SAN is to be prepared by the method described in claim 8.
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| 黄洁 等: "HPLC法测定水杨酸原料药的有关物质", 《药物分析杂志》 * |
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