Development of a rapid, multi-class method for the confirmatory analysis of anti-inflammatory drugs in bovine milk using liquid chromatography tandem mass spectrometry

A rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the simultaneous identification, confirmation and quantitation of seven licensed anti-inflammatory drugs (AIDS) in bovine milk. The method was validated in accordance with the criteria defined in Commission Decision 2002/657/EC. Two classes of AIDS were investigated, corticosteroids and non-steroidal anti-inflammatory drugs (NSAIDs). The developed method is capable of detecting and confirming dexamethasone (DXM), betamethasone (BTM), prednisolone (FRED), tolfenamic acid (TV), 5-hydroxy flunixin (5-OH-FLU). meloxicam (MLX) and 4-methyl amino antipyrine (4-MAA) at their associated maximum residue limits (MRLs). These compounds represent all the corticosteroids and NSAIDs licensed for use in bovine animals producing milk for human consumption. These compounds have never been analysed before in the same method and also 4-methyl amino antipyrine has never been analysed with the other licensed NSAIDs. The method can be considered rapid as permits the analysis of up to 30 samples in one day. Milk samples are extracted with acetonitrile; sodium chloride is added to aid partition of the milk and acetonitrile mixture. The acetonitrile extract is then subjected to liquid-liquid purification by the addition of hexane. The purified extract is finally evaporated to dryness and reconstituted in a water/acetonitrile mixture and determination is carried out by LC-MS/MS. Decision limit (CC alpha) values and detection capability (CC beta) values have been established for each compound. (C) 2009 Elsevier B.V. All rights reserved.

Biosensor immunoassay of ivermectin in bovine milk

A rapid and sensitive biosensor immunoassay was developed for determination of ivermectin residues in bovine milk. A detection limit of 16.2 ng/mL was achieved. A Biacore optical biosensor based on surface plasmon resonance was used, and a range of extraction techniques was investigated. In the final assay procedure, ivermectin was extracted with acetonitrile followed by C-8 solid-phase extraction cleanup. It was proven experimentally that 2 methods of milk storage, freezing or addition of mercury-containing compounds as preservatives, could be used without considerable change in detected concentrations (samples were fortified with ivermectin after storage). The average values for milk samples spiked at 100 and 50 ng/mL concentrations were 102.6 and 51.5 ng/mL, respectively. Extraction and analysis of 20 milk samples were performed within a single working day.

Detection of streptomycin residues in whole milk using an optical immunobiosensor

The development of an assay for the detection of streptomycin residues in pasteurized whole milk using an optical biosensor (Biacore) is reported. Streptomycin-adipic hydrazide coupled to bovine thyroglobulin was used to produce a sheep polyclonal antibody. The antibody displayed excellent cross-reactivity with dihydrostreptomycin (106%). There was no significant cross-reaction with other aminoglycosides or common antibiotics. Streptomycin was also immobilized onto a CM5 sensor chip to provide a stable, reusable surface. The developed assay permitted the direct analysis of whole milk samples (similar to3.5% fat) without prior centrifugation and defatting. Results were available in 5 min. The limit of detection of the assay was determined as 4.1 ng/mL, well below the European maximum residue limit (MRL) of 200 ng/mL. Repeatability (or coefficient of variation) between runs was determined as 3.5% (100 ng/mL; 0.5 x MRL), 5.7% (200 ng/mL; MRL), and 7.6% (400 ng/mL; 2 x MRL).

Detection of unwanted residues of ivermectin in bovine milk by dissociation-enhanced lanthanide fluoroimmunoassay

Avermectins are frequently used to control parasitic infestations in many animal species. Previous studies have shown the long-term persistence of unwanted residues of these drugs in animal tissues and fluids. An immunoassay screening test for the detection acid quantification of ivermectin residues in bovine milk has been developed. After an extensive extraction procedure, milk samples were applied to a competitive dissociation-enhanced lanthanide fluoroimmunoassay using a monoclonal antibody against an ivermectin-transferrin conjugate, The monoclonal antibody, raised in Balb C mice, showed cross-reactivity with eprinomectin (92%), abamectin (82%) and doramectin (16%). The limit of detection of the assay (mean + 3 SD), calculated from the analysis of 17 known negative samples, was calculated as 4.6 ng/mL. Intra- and inter-assay RSDs were determined as 11.6% and 15.8%, respectively, using a negative bovine milk sample fortified with 25 ng/mL ivermectin. Six Friesian milking cows were treated with ivermectin, three with a pour-on formulation of the drug and three with an injectable solution at the manufacturer's recommended dose rate. An initial mean peak in ivermectin residue concentration was detected at day 4 (mean level = 47.5 ng/mL) and day 5 post-treatment (mean level = 26.4 ng/mL) with the injectable form and pour-on treatment, respectively. A second peak in residue concentration was observed using the DELFIA(R) procedure 28 days post-treatment in both treatment groups (23.1 ng/mL injectable and 51.9 ng/mL pour-on). These second peaks were not confirmed by HPLC and must at this Lime be considered to be false-positive results. By day 35 after treatment the mean ivermectin residue concentration of both groups fell below the limit of detection of the assay. Copyright (C) 2000 John Wiley & Sons, Ltd.

Food intake, milk production, and tissue changes of Holstein-Friesian and Jersey x Holstein-Friesian dairy cows within a medium-input grazing system and a high-input total confinement system

Although interest in crossbreeding within dairy systems has increased, the role of Jersey crossbred cows within high concentrate input systems has received little attention. This experiment was designed to examine the performance of Holstein-Friesian (HF) and Jersey x Holstein-Friesian (J x HF) cows within a high concentrate input total confinement system (CON) and a medium concentrate input grazing system (GRZ). Eighty spring-calving dairy cows were used in a 2 (cow genotype) x 2 (milk production system) factorial design experiment. The experiment commenced when cows calved and encompassed a full lactation. With GRZ, cows were offered diets containing grass silage and concentrates [70:30 dry matter (DM) ratio] until turnout, grazed grass plus 1.0 kg of concentrate/day during a 199-d grazing period, and grass silage and concentrates (75:25 DM ratio) following rehousing and until drying-off. With CON, cows were confined throughout the lactation and offered diets containing grass silage and concentrates (DM ratio; 40:60, 50:50, 40:40, and 75:25 during d 1 to 100, 101 to 200, 201 to 250, and 251 until drying-off, respectively). Full-lactation concentrate DM intakes were 791 and 2,905 kg/cow for systems GRZ and CON, respectively. Although HF cows had a higher lactation milk yield than J x HF cows, the latter produced milk with a higher fat and protein content, so that solids-corrected milk yield (SCM) was unaffected by genotype. Somatic cell score was higher with the J x HF cows. Throughout lactation, HF cows were on average 37 kg heavier than J x HF cows, whereas the J x HF cows had a higher body condition score. Within each system, food intake did not differ between genotypes, whereas full-lactation yields of milk, fat plus protein, and SCM were higher with CON than with GRZ. A significant genotype x environment interaction was observed for milk yield, and a trend was found for an interaction with SCM. Crossbred cows on CON gained more body condition than HF cows, and overall pregnancy rate was unaffected by either genotype or management system. In summary, milk and SCM yields were higher with CON than with GRZ, whereas genotype had no effect on SCM. However, HF cows exhibited a greater milk yield response and a trend toward a greater SCM yield response with increasing concentrate levels compared with the crossbred cows.

Cows, milk and religion: the use of dairy produce in early societies

This review of documentary sources, particularly from Early Mesopotamia, Egypt, India and Europe seeks to show how the range of dairy products varied in different areas and to demonstrate that in many societies, cows and dairying played an important role in early religious practice. The range of dairy products consumed also varied greatly between different societies and the use of milk did not automatically imply that dairying technology was applied to its full potential. Also, in some cultures the consumption of milk was confined to certain sections of society.

Inorganic arsenic levels in rice milk exceed EU and US drinking water standards

Under EU legislation, total arsenic levels in drinking water should not exceed 10 microg l(-1), while in the US this figure is set at 10 microg l(-1) inorganic arsenic. All rice milk samples analysed in a supermarket survey (n = 19) would fail the EU limit with up to 3 times this concentration recorded, while out of the subset that had arsenic species determined (n = 15), 80% had inorganic arsenic levels above 10 microg l(-1), with the remaining 3 samples approaching this value. It is a point for discussion whether rice milk is seen as a water substitute or as a food, there are no EU or US food standards highlighting the disparity between water and food regulations in this respect.