Extractions profiles

The sfe of chlorpyrifos methyl from wheat followed by on-line Ic/gc/ecd has been investigated (93). Extraction profiles were generated to determine the maximum analyte recovery and the minimum extraction time. Using pure CO2, a 65% recovery of chlorpyrifos methyl spiked onto wheat at 50 ppb was reported. When 2% methanol was added to the CO2, the recovery from a one gram sample averaged 97.8% (n = 10, 4.0% RSD). 

Applications Albert et al. [455] have shown continuous-flow SFC-NMR spectra of five plasticisers (DEP, DNPP, DPP, BBP, DNBP). On-flow and stopped-flow pSFC-NMR of synthetic mixtures of phthalates were reported [457]. The feasibility of SFC-NMR coupling has been demonstrated with real-life applications [458]. Figure 7.20 shows a reconstruction of an extraction profile from a PVC tube [152]. The profiles of the integral aromatic proton signals between 7.2 and 8.2 ppm and the ester protons at 4.42 ppm display the relative concentration of the extracted phthalate as a function of the proceeding extraction. The structure of the extracted phthalate could be assigned to DEHP (Figure 7.21). 

Figure 7.20 Extraction profile of a phthalate from PVC. After Albert [152], Reprinted from Journal of Chromatography, A785, K. Albert, 65-83, Copyright (1997), with permission from Elsevier...

Jenke [73] studied the extractabihty of aniline, diphenylguanidine, dedenzyl-amine, and triisopropanolamine from a synthetic polyisoprene rubber similar to the material used in pharmaceutical applications. Rubber samples were autoclaved (121 °C) in contact with water or NaCl 0.9% solution for lh.Table 33 presents the concentration of each compound in solution after the extraction procedure using 2g rubber material. Extraction profiles ranged between 1.64 and 3.73 mg/L, with the exception of diphenylguanidine, whose extraction yield reached 11.76 mg/L. 

Jenke, D. R. (1997), Utihzation of extraction profiles to estimate the accumulation of extractables from polymeric materials, / Appl. Polym. Sci., 63, 843-848. 

An extraction profile is the analysis (usually by chromatographic means) of extracts obtained from a packaging component. A quantitative extraction profile is one in which the amount of each detected substance is determined. 

In both results of solubility and desorption from filter papers, diethylamine in methanol as a modifier was found to offer greater efficiency for SFE of the alkaloids than any other modifiers employed. The yields of hyoscyamine (1) and scopolamine (2) from the roots and aerial parts by SFE and conventional organic solvent extraction are listed in Tables 2 and 3. The SFE yields from both plant parts were greatly enhanced by the addition of methanol basified with diethylamine. From the results of solubility and desorption from filter paper, methanol and diethylamine/methanol (10% v/v) were much more efficient for both compounds than water and diethylamine/water (10% v/v) because of their low miscibility with C02. The extraction profile of hyoscyamine (1) when present in plant material was in good agreement with that when extracted as a pure compound. However, in the case of scopolamine (2), there... 

Figure 7.2.18 Extraction profile (contour plot) of roasted coffee using a linear pressure gradient from 85 to 220 bar...

The chloroform extraction of seven coals yielded extracts that gave unique capillary GC profiles. The coal extract profiles fell into four groups 1) BBl, BB2 Texas lignites) and MOC (Australian lignite) 2) B3 (North Dakota lignite) and WYOl (Wyoming, subbitumin-ous) 3) ALBl (Alberta, Canadian subbituminous) and 4) POWl (Ohio, bituminous coal). 

The extractables profile of the drug contact components is acceptable. 

The choice of materials available for long-term drug contact is very limited—borosilicate glass, bromobutyl or chlorobutyl rubber closures, certain inert polymers such as polytetrafluoroethylene (PTFE), tetrafluor-oethylene (TFE), and derivatives thereof, and stainless steels. Since the Code of Federal Regulations mandates that it be possible to inspect the drug product after filling, steel cannot be used as the primary drug container. In addition, polycarbonates, which would be ideal materials from durability, scratch-resistance, and cost perspectives, have very poor moisture vapor and extractables profiles. 

Quality control—The rubber component manufacturer s release criteria and drug packager s acceptance are found in this section. Also recommended is a method to monitor the consistency in composition of elastomeric components such as periodic extraction profiles. 

Acceptance criteria, test methods, and sampling plans [including qualitative and quantitative extractable profile(s)]. 

In other words, extraction procedures used in control extraction studies and for routine extraction tests of container closure system components must produce extractables profiles that can be qualitatively and quantitatively correlated with drug product leachables profiles to the proposed end of a drug product s shelf life. As stated in the regulatory guidance ... 

The ideal situation is for the extracting solvent to have the same propensity to extract substances as the dosage form, thus obtaining the same quantitative extraction profile. ... 

GC/MS analyses most often employ one of two complementary ionization processes, electron ionization (El) or chemical ionization (Cl). This is because both El and Cl are gas phase ionization phenomena and are therefore well suited to interface with a separation technique (GC) that is also accomplished in the gas phase. The extractables profiles shown in Figs. 3-5 along with the Abietic Acid GC/MS analysis shown in Fig. 1, were acquired using GC/MS with El. The El ionization process is based on the interaction of an energetic electron beam (70 eV) with neutral analyte molecules in the gas phase, producing a radical cation, or molecular ion (M+ ) that can undergo fragmentation in the gas phase after redistribution of excess... 

A) from one of the peaks in the Fig. 3 extractables profile, along with a best fit library search result... 

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