Milk, chloride determination

Milk products Determination of iodide in whole milk chloride and/or sodium in butter lactate, pyruvate and citrate in cheese... 

Helmerson 2881, and more recently Bartels 2891, determined chloride in serum by adding excess silver and then measuring the excess silver ion in the filtrate. Ezell 29°) used a similar procedure to determine chloride in plant liquors and Gutsche etal.29 determined chlorine in milk by measuring the excess silver by flame photometry. 

Methods found for the determination of diazinon in animal products also used homogenization with a polar organic solvent as the first step in residue recovery. Toyoda et al. (1990) isolated diazinon from milk via partition into methylene chloride after extraction of the milk with 70% acetonitrile in water. Based on GC/FPD, an LOD of 10 ppb and a recovery of 89% (3.8% relative standard deviation) at 100 ppb were reported. Diazinon residues in eggs were studied (Leoni et al. 1992) after blending the eggs with acetone and partitioning into dichloromethane and acetone followed by C18-silica SPE. Based on GC/FPD analysis, an LOD of 1 ppb and a recovery of 93% at 13 ppb were reported. 

Immunoaffinity cleanup was first applied in drug residue analysis for the determination of chloramphenicol in swine muscle tissue by LC (113). The lAC column was prepared using monoclonal antibodies originally developed for an enzyme-linked immunosorbent assay (ELISA) method (171) specific for chloramphenicol. Meat samples were extracted with water, and a concentrated phosphate buffer was added to the filtered extracts before immunoaffinity cleanup. A phosphate buffer was used in the washing process, whereas chloramphenicol was eluted from the column with a glycine/sodium chloride solution of pH 2.8. For subsequent LC analysis, this eluate was extracted with ethyl acetate, evaporated, and reconstimted in the mobile phase. The same analytical scheme was later successfully applied for the determination of chloramphenicol in eggs and milk as well (170, 172). 

Dissolve about 500 g. of common salt in 1,500 cc. of warm water. Heat well toward boiling and add 5 g. of lime which has been slaked and diluted to a thin paste with water (milk of lime). Add a dilute solution of barium chloride as long as the latter produces a precipitate. This is rather difficult to determine, since the liquid is turbid. The best way is to pipette off a few cubic centimeters from near the edge of the dish and... 

Other Acylglycerols. If some of the DGs in freshly drawn milk are involved in biosynthesis, it is possible that they are enantiomeric and are probably the sn-1,2 isomer. If so, the constituent fatty acids are long chain. Their configuration can be determined by stereospecific or other analyses, but it is difficult to accumulate enough material for analysis. Nevertheless, Lok (1979) isolated the DGs from freshly extracted cream as the trityl derivatives. Trityl chloride reacts selectively with primary hydroxyls. The stereochemical configuration of the DGs was identified as sn-1,2 therefore, these residual DGs were most likely intermediates of biosynthesis. If the DGs were products of lipol-ysis, they would be a mixture of 1,2/2,3 isomers in a ratio of about 1 2, since milk lipoprotein lipase preferentially attacks the sn-1 position of TGs (Jensen et al. 1983). 

The freezing point of bovine milk is usually within the range -0.512 to -0.550°C. The average value is close to -0.522°C (Dahlberg et al 1953 Davis and MacDonald 1953 Henningson 1969 Robertson 1957 Shipe 1959 Eisses and Zee 1980). It is easy to determine that lactose and chloride are the principal constituents responsible for this depres-... 

Determinative and confirmatory methods of analysis for PIR residue in bovine milk and liver have been developed, based on HPLC-TS-MS (209). Milk sample preparation consisted of precipitating the milk proteins with acidified MeCN followed by partitioning with a mixture of -butylchloride and hexane, LLE of PIR from aqueous phase into methylene chloride, and SPE cleanup. The dry residue after methylene chloride extraction was dissolved in ammonium hydroxide, and this basic solution was transferred to the top of Cl8 SPE column. The PIR elution was accomplished with TEA in MeOH. For liver, the samples were extracted with trifluoroacetic acid (TFA) in MeCN. The aqueous component was released from the organic solvent with n-butyl chloride. The aqueous solution was reduced in volume by evaporation, basified with ammonium hydroxide, and then extracted with methylene chloride. The organic solvent was evaporated to dryness, and the residue was dissolved in ammonium acetate. The overall recovery of PIR in milk was 94.5%, RSD of 8.7%, for liver 97.6%, RSD of 5.1 %. A chromatographically resolved stereoisomer of PIR with TS-MS response characteristics identical to PIR was used as an internal standard for the quantitative analysis of the ratio of peak areas of PIR and internal standard in the pro-tonated molecular-ion chromatogram at m/z 411.2. The mass spectrometer was set for an 8 min SIM-MS acquisition. Six samples can be processed and analyzed in approximately 3 hours. 

When a quantitative determination of the phosphoric acid and chlorine is required, a fresh quantity of ash is prepared from a weighed amount of the meat sample mixed with an alkali such as milk of lime, sodium carbonate, etc. The phosphoric acid and the chlorine are determined in the nitric acid solution of the ash, the former by the ammonium molybdate method, and the latter either volumetrically or gravimetrically as silver chloride. 

If sampling is not followed immediately by analysis, the sample must be treated with a preservative, but not such as to falsify the analytical results use is made of 10% potassium dichromate solution, formaldehyde, hydrogen peroxide, alcoholic solution of phenol, mercuric chloride (about 5% solution), etc., a few drops being added. The last of these preserves milk very well for several days without altering its composition or disturbing the determinations, but its poisonous character necessitates precautions. 

Ca " and so the technique is important in determining levels from fall-out in milk. Primary, secondary, tertiary and quaternary ammonium chlorides are also separated from each other by this system. 

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