Scanning electron microscopy determination of string mozzarella cheese in gastric contents.

As part of a suspected homicide investigation, a sampling of the gastric contents from the victim was forwarded to the U.S. Food and Drug Administration's Forensic Chemistry Center (FCC) for analysis of specific, selected components. The victim was known to have consumed string mozzarella cheese, as a snack, less than 24 h before his disappearance and the subsequent discovery of the body. The investigation sought to confirm or dismiss speculation the victim may have been fed a meal or eaten additional food prior to his death. Analysis of the stomach contents involved examination by stereoscopic light microscopy (SLM) and isolation, processing, and analysis of suspect materials by scanning electron microscopy (SEM). Several wax-like, off-white to cream-colored objects were noted by SLM examination and removed from the gastric contents. Through a series of fixation, sectioning, drying, and coating steps, these objects were prepared for analysis by SEM. Comparison of the suspect material with laboratory control string mozzarella cheese showed excellent correlation between the analyzed samples, confirming the suspect material from the stomach contents as string mozzarella cheese.

The relative buffering capacities of saliva and moist snuff: implications for nicotine absorption.

Commercial moist snuff products are used by placing a portion of tobacco inside the mouth between the inner cheek or lip and gum. Nicotine is absorbed into the blood stream via transfer across various oral membranes including the buccal mucosa (cheek lining). The resulting salivary pH when a given moist snuff product is placed in the mouth is an important factor for nicotine absorption because it will affect the proportion of free base nicotine that is readily available for absorption. The resulting salivary pH for a given moist snuff product will be determined in part by the relative acid-base buffering capacities of the saliva and moist snuff, as well as the pHs of the saliva and moist snuff prior to coming in contact with one another. In the current study, the acid-base buffering capacities (mu eq/g) of a series of commercial moist snuff products were determined and compared to the acid-base buffering capacity for unstimulated, whole human saliva. The buffering capacities of the moist snuff products were determined to be 10-20 times higher than the buffering capacity of human saliva. The resulting salivary pH ranges after contact between an artifical saliva and the various moist snuff products were also determined; the results were used to predict the proportion of free base nicotine that can be expected to occur in the mouth during the first few minutes of product use. These studies provide a basis for examining and understanding the effects that moist snuff product pHs and buffering capacities may be expected to have on nicotine absorption.

Detection of adulteration of locust bean gum with guar gum by capillary electrophoresis and polarized light microscopy.

Capillary electrophoresis (CE) and polarized light microscopy (PLM) were utilized in the detection of the adulteration of locust bean gum with guar gum. For CE analyses, standards of locust bean and guar gums were extracted with 30% CH3CN, removing the residual proteins from the gum matrix. A 8.75 mM NaH2PO4-20.6 mM Na2B4O7 buffer, pH 9, was used to separate these proteins and to identify marker proteins that were present in the guar gum. These markers did not co-migrate with components in the extracts of mechanically processed locust bean gum, and are used as indicators of adulteration. Using PLM with toluidine blue and iodine staining techniques, unadulterated locust bean gum samples were distinguished from mixed samples through the differential staining of components in locust bean versus guar and tara gums. These experiments in the use of CE and PLM provide orthogonal and complementary methods for the verification of 'true' positives and the elimination of 'false' positives.

Detection of counterfeit and relabeled infant formulas by high-pH anion-exchange chromatography-pulsed amperometric detection for the determination of sugar profiles.

High pH anion-exchange separation with pulsed amperometric detection (HPAE-PAD) is used to characterize various milk-based, soy-based, and protein hydrolysate infant formulas based on carbohydrate profiles. Counterfeit and relabeled formulas are compared to authentics. Figures of merit are shown for glucose, fructose, lactose, sucrose, and maltose.

A false report of product tampering involving a rodent and soft drink can: light microscopy, image analysis and scanning electron microscopy/energy dispersive X-ray analysis.

The "Pepsi Tamperings" of 1993 resulted in a large number of cases involving foreign objects reportedly found inside canned soft drinks. Although the majority of cases involved medical syringes and metallic objects, one case involved the report of a mouse found inside a can of Caffeine-Free Diet Pepsi. Using light and polarized light microscopy and computer-assisted image analysis, trace evidence and tooth structure from the suspect mouse were matched to scratches and indentions on the suspect can. Scanning electron microscopy and energy dispersive X-ray analysis were used to compare and match particles of gnawed metal from the lid of the suspect can to other particles recovered from the muzzle and stomach of the suspect mouse. The forensic analyses in this case proved the mouse could not have been canned in the soft drink product and refuted the defendant's sworn statements.

Determination of ephedrine compounds in nutritional supplements by cyclodextrin-modified capillary electrophoresis.

Capillary electrophoresis was utilized for the separation, identification, and quantitation of ten stereoisomers in the ephedrine family. Chiral discrimination was accomplished through the use of hydroxypropyl-beta-cyclodextrin, and separation was enhanced at pH 2 in the presence of tetramethylammonium chloride and sodium dodecyl sulfate. Calibration plots of the ephedrines were linear over the range 4-100 micrograms/ml. This method was used in the analysis of nutritional supplements that contain Ma Huang, a Chinese herbal preparation that is made from plants in the genus Ephedra.

Chemical profiling of pharmaceuticals by capillary electrophoresis in the determination of drug origin.

Capillary electrophoresis has been utilized to detect trace components in bulk pharmaceutical products, with emphasis on the identification of differences among manufacturers that can be used for source verification in suspect/counterfeit cases. Micellar electrokinetic capillary chromatography with sodium dodecyl sulfate was used in the analyses of beta-lactam antibiotics. The aminoglycoside clindamycin phosphate and the macrolide erythromycin stearate were analyzed using borate buffers with direct UV detection. Methyl-beta-cyclodextrin was used as a buffer additive in the erythromycin studies. Determination of product potency using peak area ratios has been demonstrated for ampicillin and clindamycin phosphate.

Forensic investigation of gentamicin sulfates by anion-exchange ion chromatography with pulsed electrochemical detection.

Many methods exist for the separation of gentamicin C complex components, C1, C1a, C2 and C2a. In an investigation of possible counterfeit suppliers of gentamicin sulfate, a new method utilized high-pH anion-exchange separation on a carbohydrate column, with pulsed electrochemical detection on a gold electrode. Component ratios and the presence and/or absence of additional peaks were used to link or dissociate forensic samples.

Practical applications of element-specific detection by inductively coupled plasma atomic emission spectroscopy and inductively coupled plasma mass spectrometry to ion chromatography of foods.

Three practical examples are presented to demonstrate the utility of element-selective detection for ion chromatography (IC). The determination of As species in a liquid health food supplement by IC with inductively coupled plasma atomic emission spectroscopy (IC-ICP-AES) is shown to confirm results obtained for total As. IC-ICP-AES is also used to investigate the identity of an unknown peak in a sample of shrimp commercially treated with tripolyphosphate. Finally, results are presented for the determination of residual bromate in baked goods by IC with inductively coupled plasma mass spectrometry detection.

Quantitation of gentamicin sulfate in injectable solutions by capillary electrophoresis.

The results presented in this communication establish the use of capillary electrophoresis as a tool in the analysis of injectable solutions containing the antibiotic complex gentamicin sulfate. The utilization of a borate buffer leads to the separation of the individual components and their visualization by direct UV detection. This rapid and straightforward procedure yields qualitative and quantitative information simultaneously, and could be utilized as an alternative to the multiple assays required by current US Pharmacopoeia protocols.

Arsenic speciation by ion chromatography with inductively coupled plasma mass spectrometric detection.

Four As compounds were successfully separated and detected by single-column ion chromatography with inductively coupled plasma (ICP) mass spectrometric detection. The mass spectral interferent ArCl+ was reduced by chromatographically resolving chloride from the negatively charged arsenic species. Determination of four As species was investigated in urine, club soda and wine. Detection limits of 0.16 ng of As(III), 0.26 ng of As(v), 0.073 ng of dimethylarsinic acid (DMA) and 0.18 ng of methylarsonic acid (MMA) in wine were obtained. Sensitivity was further improved by using an He-Ar mixed gas ICP as the ionization source. However, the intensity of the ArCl+ interference was also increased using this plasma. Detection limits of 0.063 ng of As(III), 0.037 ng of As(v), 0.032 ng of DMA and 0.080 ng of MMA in club soda were achieved using the He-Ar plasma source. Similar limits of detection were found in urine and wine.

Purified reference diets for weanling rats: effects of biotin and cellulose.

Standardized purified diets limited to required nutrients are needed for nutritional and toxicological studies. In the present study, we formulated a biotin- and cellulose-free diet of reproducible mineral composition (diet A), based on diet AIN-76, and fed it to weanling Long-Evans rats for 3 wk. Inductively coupled argon plasma atomic emission spectrometry was used to determine Ca, Cu, Fe, K, Mg, Mn, Na, P and Zn in liver, duodenum, kidney, spleen and femur. Results were compared with those obtained with rats fed biotin- and/or cellulose-supplemented variations of diet A, diet AIN-76 and diet NIH-31 (an open-formula stock diet). Weanling rats grew slowly and steadily on purified diet A. Growth rates increased when diet A was supplemented with biotin and cellulose. In general, differences among tissue mineral levels in rats fed diet NIH-31 and those fed diet AIN-76 were more pronounced than those among groups fed our purified diets. Values for hemoglobin and hematocrit were significantly lower in rats fed all purified diets than in those fed diet NIH-31. Diets A + biotin, A + cellulose and A + cellulose + biotin appear satisfactory as reference diets for measuring mineral interactions at near-requirement levels as well as effects of fiber on mineral utilization or for studies on vitamins whose endogenous synthesis may be influenced by dietary fiber.

Trace element studies in weanling rats: maternal diets and baseline tissue mineral values.

The initial nutritional status of experimental animals can influence their response to subsequent dietary regimens. In the present study, we determined the variations in minerals in diet NIH-31, a breeding colony stock diet, and in tissues of weanling rats nursed by dams fed this diet. Inductively coupled plasma-atomic emission spectrometry (ICP-AES) was used to determine nine elements (Ca, Cu, Fe, K, Mg, Mn, Na, P and Zn) in diet and in liver, kidney, spleen, duodenum and femur from 22- to 26-day-old rats. Wet digestions were performed in mixtures of nitric, perchloric, and sulfuric acids (diets and soft tissues) or nitric and perchloric acids (femur). Solution concentrations ranged from less than 25 ng/ml for the trace elements to greater than 100 micrograms/ml for the major elements. Large variations in mineral content were found between batches of commercially prepared NIH-31 diet; relative amounts of Cu, Fe, Mn and Zn varied markedly. Significant differences in concentrations of major and trace minerals in liver, kidney, spleen and duodenal tissue were found among groups of weanling rats obtained from the same supplier at different times. Mn was readily quantitated in all tissues except spleen, where it was below detection limits. The precision obtained with the ICP-AES methodology has significant advantages for establishing variations in tissue mineral levels.

Hydride generation and condensation flame atomic absorption spectroscopic determination of antimony in raw coffee beans and processed coffee.

A method was developed for determining Sb at nanogram per gram levels in raw coffee beans and processed coffee. The procedure uses either total acid digestion or extraction with 6M HCl followed by hydride generation/condensation with subsequent revolatilization of stibine (SbH3) and detection by flame atomic absorption spectroscopy. The lowest quantifiable level, based on a 2 g (dry weight) sample, is 2 ng Sb/g. The results of recoveries on spiked samples, precision studies on composited coffee samples, and the analysis of National Bureau of Standards Standard Reference Materials demonstrate the reliability and accuracy of the procedure. Sb concentrations in coffee samples were verified by neutron activation analysis and inductively coupled plasma atomic emission spectroscopy. Advantages of the method compared with the AOAC colorimetric procedure and hydride generation without condensation are discussed.