Stainless steel coupons for cleaning validation

We tested several of the most common slip agents, wetting agents, and packaging materials used in the industry: erucamide, oleamide, stearamide, talc, polyisoprene, and polyethylene. Erucamide, oleamide, Figure 5 and stearamide are the most commonly used slip agents in the pharmaceutical industry and life sciences industries. Because they are insoluble in water and buffers, they tend to float at the liquid surface, aggregate at the air—liquid interface, and adhere to the tank side wall.

The coating process consisted of dispensing approximately 4 ml of samples onto the coupon with a plastic transfer pipette, and then spreading the sample over an approximately cm2 area with the pipette. The hardest-to-clean condition was when the slip agent was dissolved in methanol or ethanol and then mixed with the buffer. Coated coupons were conditioned five ways:. Because condition 5 was hardest to clean, we chose it as our test model.

We evaluated the following cleaning agents to determine the most suitable chemistry for removing erucamide, oelamide, and stearamide residues from the air—liquid interface Table C :.

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Cleaners formulated with sodium hypochlorite or hydrogen peroxide use oxidation as the cleaning mechanism. Oxidation cleaves high-molecular-weight molecules into smaller molecules, which are more susceptible to removal by other cleaning mechanisms, such as emulsion, solubility, and hydrolysis. Repeated use of oxidative cleaning agents at high concentration and temperature may discolor stainless steel, so these are generally used for periodic cleaning.

When assessing the effect of the air—liquid interface residue on the quality of the next product or batch, one should ask the questions shown in Table D. The rings appeared at multiple levels in the tank and were black in color. The blended product was water soluble, so purified water was used to clean the tank between product batches.

After visual inspection of the tank, the air—liquid interface rings were wiped and scraped, and the residue was submitted for material analysis; a wipe sample of a black gasket was also submitted Figure 7.

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The results of the scraped material were somewhat inconclusive as to its source, due to the opacity of the black particulates. However, Fourier transform infrared spectroscopy FTIR results from the gasket and tank ring wipes appeared similar. Infrared spectroscopic data were collected between 4, cm-1 and cm-1 neat. A background spectrum was collected using the blank ATR diamond cell. Results The FTIR gasket spectra carbon black filled and the black scraping material produced skewed baselines.

Cleaning Verification Using Direct NIR Imaging

Carbon black filled types of materials are difficult to analyze by spectroscopic methods because of their very high absorption rates and their propensity to scatter infrared light. Figure 8 shows the spectrum of the gasket; Figure 9 shows the spectrum of the black scraping from the ring in the tank. Note that although the spectra are not exactly the same, there are similarities in some absorbance bands and the baseline slope. Spectra of the wipe material clean spot and black residue on the wipe were collected independently. Spectral subtraction was used to determine the black residue on the wiping material.

The spectra from gasket and tank ring wipes Figure 10 appear to be fairly similar after subtraction of the wipe material. The tank rings contained residue from the black EPDM gaskets. Water-only cleaning was not sufficient to remove the hydrophobic residue, which allowed it to build up on the tank as visible residue. The solution was filtered into a storage tank where there were no observed rings.

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Further testing should be done to identify the residue and assess its effect on the product. Gaskets were replaced and the tanks were cleaned with a combination of manual cleaning brush from the manway and automated cleaning using a spray device with a formulated alkaline cleaning agent containing surfactants.


The tanks and gaskets were also monitored more closely to determine if the gaskets should be replaced more frequently. A biopharmaceutical manufacturer was observing air—liquid interface rings in its sodium chloride buffer tanks. The sodium chloride arrives as large clumps in polyethylene containers with a polyethylene bag liner Figure The clumps are broken up by the operators while in the container prior to preparing a sodium chloride solution.

The buffer tanks are cleaned with water between batches.

Laboratory studies to investigate residue ring cleaning and prevention were conducted in parallel with field trials and analytical residue testing. Procedure Laboratory testing consisted of two parts:. Results While the coupons were visually clean, those cleaned only with water failed the water break free test after only one soiling and cleaning cycle Figure The water break free failure was not produced on stainless steel when cleaned with 0.

Analytical testing of the air—liquid interface rings demonstrated trace polyethylene residue, most likely from the raw material packaging. The results did not confirm conclusively that the residue observed in the laboratory studies was polyethylene, however. These laboratory studies demonstrated that the sodium chloride contained a water-insoluble hydrophobic residue that remained on the surface when cleaned only with water. This residue could continue to build up on the surface and result in a visual failure or reduce the efficiency of subsequent cleaning, sanitization, or stainless steel maintenance.

A low-concentration alkaline cleaning agent with surfactants appeared to remove this hydrophobic residue when used after each cleaning. Periodic cleaning of the surface with a low-concentration alkaline cleaning agent after the residue develops to a visual failure was not evaluated during this study. This article reviewed common buffers used in pharmaceutical and biopharmaceutical manufacturing processes.

Based on solubility and benchtop cleaning trials, water should be effective at removing theses residue. However, trace components from the packaging, raw materials, gaskets, diaphragms, tubing, etc. Identifying the ring components is the first step in determining whether the residue is intrinsic e. Laboratory studies have been effective at providing a course of action in some cases, but simulating the air—liquid interface residue without having identified the residue remains a challenge.

Please enable JavaScript to access the full features of the site or access our non-JavaScript page. Issue 4, Previous Article Next Article. From the journal: Analytical Methods.

Cleaning validation – MOC sample coupons unavailable? – Blue Hatch Consultancy Ltd

Validation of cleaning of pharmaceutical manufacturing equipment, illustrated by determination of cephradine residues. You have access to this article. Please wait while we load your content Something went wrong.

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Try again? Cited by. Back to tab navigation Download options Please wait Article type: Paper. DOI: Download Citation: Anal. Validation of cleaning of pharmaceutical manufacturing equipment, illustrated by determination of cephradine residues S. Sajid, M. Arayne and N. Sultana, Anal. Search articles by author S.

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