Diclofenac - Science topic

J. N. O. Ezeugo first check solubility (ALCOHOLIC) and accordingly you should prepare homogeneous extract, you may try to chloroform:methanol:glacial acetic acid (6:3:0.5:0.5 v/v). All the best

Back to your original question (and I am done with this thread)... You observed a small (tiny) difference in Rt from small changes you made to the mobile phase composition. No worries, this is normal because no two columns are the same and each may interact to a different degree (or none at all) when you make small changes to the mobile phase composition. Try 20 different C18 columns and you may find some show no change at all, some do. Pick and choose the one that you want for the application (this is what we do in analytical laboratories). The reason for the observed change (change, not "drift") is due to multiple interactions of the solute on the surface of the support. Hard to say if it is electronic or ionization in nature, but it is so small, practically, it does not matter. All chromatographers are familiar with this (no need to 'explain it'). Run enough samples and you will see it. In fact, the one thing that they might question is why you would use a mobile phase of just ammonium formate without an acid (e.g.formic). Why not use a buffer? For LC-MS applications, most would benefit from such a solution to promote ionization and maybe change the separation factor too (depends on samples).

Usually, the university owns the rights to publish dissertations. Your university will upload your dissertation to the university's repository. Some journal might publish dissertations if they have an agreement with certain universities.

There are many sources of Sodium, so you do not want to validate or follow Sodium by either AAS or flame emission at 589 nm. Dicloflonac is your active ingredient and has a physiological response, so this is what you use in cleaning validation (use HPLC since it is more sensitive). For validation follow the guidelines of ICH Q2 and use HBEL (health based evaluation limits based on toxicity to calculate your minimum safety concentration).

please find it here: https://pubchem.ncbi.nlm.nih.gov

I'm not an expert in toxicology. But every chemist is well aware that methanol itself is very toxic. It would be more fun to use ethanol

Dear Sara Napolitano ,

Indeed, though they look misleadingly professional they are not. “Austing Publishing Group” is mentioned in the Beall’s list (https://beallslist.net/) and numerous disturbing things are associated to them: http://flakyj.blogspot.com/2017/08/austin-publishing-group.htmlFurthermore:

After all those years no serious indexing (https://www.austinpublishinggroup.com/indexing.html), as a matter of fact DRJI is a well-known example of a misleading metrics (https://beallslist.net/misleading-metrics/)

Looking at the specific journal, they prominently mention impact factor a 2.1 (https://www.austinpublishinggroup.com/clinical-case-reports/) which is to say the least misleading because they are not indexed in Clarivate’s SCIE (which can be checked here )

They struggle to get enough submissions and mostly likely are desperately need content (https://www.scilit.net/journal/761969)

In other words, this ‘publisher’ is using questionable practices and unlikely will respond to your request to withdraw/remove your paper. It would be a good thing if the Tumori journal (https://journals.sagepub.com/home/tmj) is willing to publish the paper (despite the fact that they are fully aware of the problem). Though this would be justified it is unfortunate that the ’law’ more or less protects these types of fraudsters in terms of copyright etc. and seems powerless to punish those who do not follow ‘the rules’. In general, this is the current status: “If I publish an article in a predatory journal, can I republish it elsewhere? Sadly, dual publication is a breach of publication ethics whether the original article is published in a predatory journal or a legitimate one. The best course of action is to build on the original article with further research so that it is substantially different from the original and publish the subsequent paper in a legitimate journal.” (https://blog.cabells.com/tag/predatory-journals/page/2/).

Best regards.

See for related topics:

Why do you say so?

Diclofenac is a NSAID! So, if RO/NF membrane separation process is efficient for NSAIDs, it should efficient for diclofenac as well!

Also check http://lib.tmd.ac.jp/jmd/0504/09_Nakanishi.pdf

Thanks

Amen Ekhosuehi Some use "initial pH" where the initial pH is adjusted with HCl or NaOH

while others use buffers Tris and phosphate at low ionic strength to prevent competition from the adsorbate.

but accoridng to

ionic strength of the buffer "reduces biosorptive removal of adsorptive pollutant by competing with the adsorbate for binding sites of biosorbent."

It is a case by case basis. if your target is metal than pH drift during sorption (releases H+ ion for instance) may affect sorption as the metal may have limited solubility at certain pHs.

(Fig. 5)

and

In short, maintaining pH whilst preventing unwanted consequences is the "Elephant in the room" in the biosorption process

Either look for the unit cells (a, b, and c) from the X-ray crystallographic studies in the literature, or draw the compound in a molecular dynamic software such as Mopac, Gaussian, ... and after getting the equilibrium structure calculate the size form the bond length.

1. 45% acetonitrile + 55% water(0.01% acetic acid)

2. Methanol and 0.1% formic acid in water (75:25, V/V)

3. 10 mM formic acid and acetonitrile (40/60)

Dear all, please check the following document. My Regards

Thank you for the reply, Professor

Hello Maurizio Cuomo , you can measure a lot of micropolltants with HPLC. My researches deals intensively with pharmaceuticals. You are welcome to have a look at my paper, then you will see which eluents, columns etc. I normally used.

If you want to work with spiked samples, of course it depends on which detection-system you use. It is generally recommended to measure the water samples unspiked, almost as a blind sample, so that you can see exactly what differences are between spiked and unspiked samples.

OK

I agree with Dr. Shreenath's answer that qmax would be good fit with the b value of the Langmuir model.

Keerthanan Santhirasekaram thank you

Hi Janina

During my study of diclofenac, there were very large concentrations of diclofenac present in treatment plants that reached milligrams per liter and not micrograms per liter for use in some industries. diclofenac is used as a medicine for diseases, but, the increase in concentration in the human body has an adverse effect on human health such as its effect on kidneys and others, And prevent the use of veterinary medicine, its presence in the sewage system is not fully completed in conventional treatment. The treatment was achieved only 40-60% due to its physical and chemical properties, polarity, water solubility, stability, microbial resistance and bioaccumulation in the series Food

Thank u all for the suggestions

HSA has only one Trp. And dansyl group is a perfect quencher. So, you can preferentially excite the Trp by using 295 nm light and do the FRET calculation. FRET is called the spectroscopic ruler. The FRET distance will tell you how far away from the Trp each of the ligand are binding. From that you can deduce which one is binding to site I and which one is binding to site II.

Use a suitable solvent to mix them and then coat it on a substrate to obtain a thin film. The thickness of your film depends on the polymer concentration...

The data of the metabolite of diclofenac you need as the following with the best wishes

Solid phase extraction

You clean and preconcentrate

It is the best way to clean dirty samples

Hi, read this article.

So appending the answer above, you need 14,5 moles of oxygen per 1 mole of this compound. Often the theoretical value does not correnspod to measured COD.

Secondly, remember that, depending on your AOP process the machanism is different - the injected oxidant is nor reacting directly with the compounds - it is AOP, so you try to produce hydroxyl radicals.

But still, reporting the oxidant amount added in respect to COD (as a ratio) is a good approach.

You can check this papers,

regards,

G

Dear Wolfram

There are numerous methods for diclofenac analysis from standards, formulations and from numerous biological fluids covering both LC-UV and LC-MS methods so scouting for conditions is not required, the LC methods are already reported.

For LC-MS methods where ESI ionisation is used care should be taken with the use of TFA and should be avoided if positive mode ionisation is being done as it scavenges the positive ions reducing the sensitivity of the method and if used should be less than 0.1%

Diclofan is not a addiction drugs but I think the patient habits specially suppositoy as a roat of administration  is a main cause of addiction as your description!!!

Thanks Dr. Valerii for your answer

dear doctor,

ucan very well use the diclofecnac sodium in your study

Alyona, if you have TOC of raw wastewater of say a few hundred mg/L, and to that you add a few mg/L of the pharmaceuticals, the difference in TOC is very low. Depending on the precision of your analysis (which, in turn, depends on your equipment and its current condition, "freshness" and precision of calibration curve, solution preparation, and so forth), the difference of TOC you should expect from adding the pharmaceuticals might as well fall under the measurement precision.

In figures: let us assume that you have a modelled municipal wastewater with TOC of 500 mg/L, as mentioned by Henrik. Then, you add say 10 mg/L of ibuprofen (IBP): its molar mass is 206, and from this and its formula (C13H18O2) we can calculate that the share of carbon is 12*13/203 = 0.75, so 10 mg/L IBP should equal 7.5 mg/L TOC. And this is 1.5 % of your initial solution TOC! This may be well under the deviation you get between parallel samples, or at least something very comparable. Should you add not 10, but 1 mg/L IBP to the mentioned matrix, that would make up 0.15 % of the initial TOC, respectively - this will certainly be within the measurement precision limits.

To sum up, you can see either a decrease or increase in TOC (and you say it was insignificant decrease) upon the addition of IBP or something else to simulated wastewater matrix, but the reason behind this can be simply the measurement precision: as you said, you had just one trial. If you make more measurements, most likely you will see the results "floating" around that what you get for your model wastewater.

There is a demand on surfacewater in the EU as derivative of the water framework directive to keep below 100 ng/L. depending on the dilution of wastewater into the surface water this will have implications on wastewater.

E.g. if a surface water contains 50% treated wastewater and th 100 ng/L apply, then the wastewater effluent must keep below 200 ng/L. If you have only 10% wastewater in the surface water you are OK as long as the wastewater keeps below 1000ng/L

 Dear Hatem,

The septic shock is most likely the result of kidney infection because of obstruction by the stone and diclofenac does not cause septic shock this way.

Diclofenac can influence the outcome from septic shock, by contributing to acute kidney injury in the context of septic shock, or by causing a separate problem such as perforated stomach ulcer which could lead to septic shock, but that is almost certainly not the case here (based on the details you describe).

The 

maybe this will help you too

On page 5 of this MSc thesis(at University of North Carolina, Wilmington, U.S.A) , you will find the procedure to prepare diclofenac acid from its sodium salt. It is an easy procedure which gives the free acid in solid form.

Best wishes for success in your research.

I would suggest this systematic review by Cochrane Database Syst Rev

Holdgate A, Pollock T. Nonsteroidal anti-inflammatory drugs (NSAIDs) versus opioids for acute renal colic. Cochrane Database Syst Rev. 2005(2):CD004137.

Briefly

A Cochrane review concluded that both NSAIDs and opioids provide effective relief from renal colic. Some evidence suggested that NSAIDs were more effective, and that opioid use was associated with more adverse effects, mainly vomiting. Trials included in this Cochrane review did not directly assess gastrointestinal bleeding or worsening of renal function. However, these potential adverse effects were infrequent in the Cochrane review and in a previously published meta-analysis of NSAIDs for renal colic ( Labrecque M, Dostaler LP, Rousselle R, Nguyen T, Poirier S. Efficacy of nonsteroidal anti-inflammatory drugs in the treatment of acute renal colic: a meta-analysis. Arch Intern Med. 1994;154(12):1381–1387).

Treatment harms are important, and trials designed to show if NSAIDs pose a risk in kidney stone treatment would be helpful. However, based on a paucity of evidence that NSAIDs are harmful in most patients with kidney stones, physicians should not exclude NSAIDs as an option for relieving renal colic.

These following comments were from "Am Fam Physician. 2012 Jun 15;85(12):1127. by CHARLES CARTER, MD, FAAFP"

Best regards,

Wisit

dear muruthi 

thank you for reply, but i want to know a powder type material density.

Yes it should be banned for vet use and for humans its one of the best NSAID drugs and widely use in tablets,injections and topical creams.

When working with compounds having a very pH sensitive retention time in a gradient system you might want to try adding the same amount of ammonium acetate to your organic phase to ensure a stable pH throughout your gradient. When doing so, methanol or other protic organic solvents might be more suitable than acetonitrile. Furthermore, a higher concentration of ammonia acetate (up to 25 or 50 mM depending on your organic phase) can increase your buffering capacity and better stabilize your pH. Be sure that your pH of the mobile phase is not in close proximity to the pKa of your compound so that your compound will not switch back and forth between ionized and non-ionized forms. Does the solvent of your sample resemble your starting mobile phase composition? Too much of organic solvent in your sample can cause severe chromatographic problems. Do you have any knowledge of the stability of your compound? As far as I remember diclofenac might be light sensitive. What about your storage conditions? Some compounds don't like to be repeatedly freezed and thawed. Some compounds are better off not to have water in the stock solution to prevent hydrolysis. If you have water in your working solutions you might want to consider to freshly dilute them on a daily basis from the water free stock solution.

As for cleaning your HPLC from bacteria/algae you might want to try purging with isopropanol but take care of the high viscosity and resulting back pressure. Also you could reduce bacteria/algae growth by using light protected containers (e.g. brown glass bottles).

Good luck!

Dear Mr Cojacuru, it is possible to determine sodium diclofenac by direct UV-VIS in water. Pharmacopeia describes HPLC or potentiometric titration. However, potentiometry is only possible for pure sample (>99%). This is because excipients are Lewis base on acetic acid/acetic anidride medium and titrated by perchloric acid. Besides if you use glass electrode is necessary to change the KCl electrolyte from water to methanol. In this case, water is also a Lewis base in organic medium being also titrated. The article that I suggest (follow in attachment) uses UV-VIs. The principle is very simple. Sodium diclofenac is sparingly soluble in water, but in low concentration is completely soluble. This concentration is near to range of the spectrophotometer response. However, the excipientes when the sample is diluted in water are "insolubles". The measure is made at 276 nm. Another possibility is to use catalytic thermometric titration in organic solvents. I hope to have helped you.

Then it might be probably due to the the sodium ion ...... or it might be the incompatibility with the excipient or the vehicle , plz check the quality of the water also .

J Int Med Res. 1986;14(2):95-100.

Diclofenac sodium versus acetylsalicylic acid: a randomized study in febrile patients.

Bettini R, Grossi E, Rapazzini P, Giardina G

Methods Find Exp Clin Pharmacol. 1983 Oct;5(8):579-80.

[Imadyl: gastric irritation in comparison with acetylsalicylic acid, indomethacin, piroxicam and diclofenac-Na].

[Article in German]

Brendl K, Bruhn R, Ganote DP, Lücker PW, Scholz HJ

[Stomach tolerance of non-steroid anti-rheumatic agents. Studies on gastric irritation caused by carprofen in comparison with acetylsalicyclic acid, indomethacin, piroxicam, and diclofenac].

Bruhn R, Brendl K, Ganote DP, Lücker PW, Scholz HJ.

As you can see only old studies are available. Recent experiences are predominantly dedicated to compare gastric toxicity between anti-COX2 and anti-COX1 non steroidal anti-inflammatory drugs. The limit of the above reported studies is that they do not consider H. pylori status, which is relevant for ulcer development.

It is important to known the quantum yield value, this form we known if the emission is due fluorescence or phosphorescence, so the absorption or excitation energy can be only as a trigger step if the phenomenon it is phosphorescence.

Generally most of NSAIDs can cause peptic ulcer at different dose. Ex.: Aspirin (200mg/kg), Ibuprofen, Indomethacin (20mg/kg), etc.

There are few more agents which can be used to induce peptic ulcer like Ethanol, Cysteamine.

One advice I would like to give choose the model according to probable mechanism of your drug/agent.

Is there any method for HPLC analysis of diclofenac sodium patchapplication?

What is the analysis procedure for magniesium -calicium carbonate as antacid preparation?

Two questions here? Please be more specific with your problem