RP-HPLC测定N-苯基-2,6-二氯苯胺合成反应的终点

目的:建立高效液相色谱法测定N-苯基-2,6-二氯苯胺合成反应的终点.方法:采用Shim-Pack CLS-ODS色谱柱(15cmX6mm,5μm);甲醇-水(80:20)为流动相;紫外检测波长254nm.结果:N-苯基-2,6-二氯苯胺与2,6-二氯苯胺在3.22～9.67μg范围内呈良好的线性关系.平均回收率为100.6%,RSD二1.8%.结论:方法简单可行,迅速准确.     

Determination of bisphenol A in, and its migration from, PVC stretch film used for food packaging

Bisphenol A (BPA) is used as an additive in polyvinyl chloride (PVC) products, including stretch films used for food packaging. The BPA contents were investigated of several brands of stretch film bought locally but marketed internationally or throughout Spain and which were presumably produced at different manufacturing plants. Their major components were identified by FTIR (Fourier Transform Infrared Spectrometry) and horizontal attenuated total reflectance, and the migration of BPA from these materials into the standard European Union food simulants was determined by high-performance liquid chromatography (HPLC) using both fluorescence (FL) and ultraviolet (UV) detection, the identity of the analyte being confirmed by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS). The two HPLC detection methods had different detection limits (30 μg l^-1 for UV, 3 μg l^-1 for FL), but afforded virtually identical BPA determinations for the samples tested. BPA contents ranging from 40 to 100 mg kg^-1 were found in three of the five PVC-based films analysed, and a content of 500 mg kg^-1 was found in a fourth; for these determinations, extraction into acetonitrile was used. In standard tests of migration into water, 3% acetic acid and olive oil over 10 days at 40°C, migration from a given film was in all cases greatest into olive oil. Migration from the films with non-zero BPA contents ranged from 3 to 31 μg dm^-2, values higher than those reported for many other food-contact materials, but lower than the European Union specific migration limit for BPA. PVC stretch film nevertheless may make a significant contribution to contamination of foodstuffs by BPA, and should be taken into account in estimating BPA intake or exposure to this substance.     

Aflatoxin M 1 contamination in commercial samples of milk and dairy products in Kuwait

As part of the programme on monitoring of environmental contaminants in food stuffs in Kuwait, 54 samples of fresh full cream and skimmed milk, powdered milk, yoghurt, and infant formula were analysed for aflatoxin M 1 (AFM 1 ) by HPLC following sample clean up using immuno-affinity columns. Of samples, 28% were contaminated with AFM 1 with 6% being above the maximum permissible limit of 0.2 μg l -1 . Three fresh cow milk samples collected from a private local producer showed the highest level of 0.21 μg l -1 AFM 1 . There was no contamination with AFM 1 in powdered milk and infant formulas. These results show the necessity of a survey involving a larger number of milk and its products and suggest that presently the contamination of milk and milk products with AFM 1 does not appear to be a serious health problem in Kuwait. Nevertheless, a continuous surveillance programme may be warranted to monitor regularly the occurrence of aflatoxins in the animal feeds responsible for current limited contamination and to note rapidly any worsening in the situation that may depend on market changes or on unfavourable climatic developments.     

Occurrence of T-2 toxin in processed cereals and pulses in Turkey determined by HPLC and TLC

The purpose of this study was to investigate the T-2 toxin level of contaminated cereal and pulse products in Turkey. T-2 toxin was detected using high performance liquid chromatography (HPLC) with UV detection at 208 nm and thin layer chromatography (TLC) was used for confirmation of the T-2 toxin-contaminated samples (> or = 1 ppm). The recovery was 93 +/- 3.3% (SD 3.29, n = 5) for chickpea spiked with a known amount of T-2 toxin (1 ppm). The detection limits for T-2 toxin for HPLC and TLC were 25 ng per injection and 50 ng per spot, respectively. A total of 50 commercially available cereal and pulse product samples, collected from markets and street bazaars, were analysed. Incidences of T-2 toxin detected in cereal and pulse products were 23.5% and 31.2%, respectively and the maximum detected amount was 1.9 ppm in a sample of dried beans. The incidence of toxin-contaminated specimens is not so low relative to the volume of specimens produced.     

Sulphonamide residues in eggs following drug administration via the drinking water

The aim was to determine concentrations of sulphadimidine (SDM) and sulphadimethoxine (SDT) in eggs following oral administration through drinking water for 5 days (0.5g^-1 for SDT, 1 and 2gl^-1 for SDM). Residues of sulphonamides in albumen and yolk were monitored by high-performance liquid chromatography with UV detection. The limit of quantification was 0.005 μg g^-1 for the two egg components. The results indicate that 0.9-1.4% of the dose administered was deposited in eggs. Maximum concentrations in albumen were much higher than those in yolk. More than 75% of the overall sulphonamides detected in eggs was concentrated in the albumen. The residue levels declined below the limit of quantification within 12-20 days for albumen and 14-15 days for yolk after treatment was discontinued.     

SIMULTANEOUS DETERMINATION OF α, β AND ISO-α ACIDS IN HOPS AND HOP PRODUCTS

A method for the simultaneous analysis of α, β and iso-α acid in hops, hop extracts and isomerised hop extracts is described. It is based on the use of reversed phase high performance liquid chromatography and quantitative evaluation of the hop compounds is carried out with a computing integrator. The isomerisation reaction can be examined in detail, particularly in connection with the production of hop derived haze forming compounds in isomerised hop extracts used for post fermentation bittering.     

Hydrolysis of freshly prepared wheat starch fractions and commercial wheat starch using α-amylase

The enzymic hydrolysis of commercial wheat starch and freshly prepared wheat starch fractions was studied in batch and flow systems. Fresh starch was prepared by wet separation of wheat flour into starch milk and gluten, followed by processing the starch milk using a serially connected hydrocyclone system to produce underflow and overflow streams. The underflow stream consisted mainly of the larger (> 30 w m) granules, while the overflow stream contained only the smaller (< 10 w m) granules. In batch system, the hydrolysis behavior of wheat starch fractions was investigated under the action of Sigma f -amylase ( Bacillus licheniformis ), either as soon as they were prepared or after spray drying. The two fractions of fresh wheat starch showed different hydrolysis behavior, the difference getting larger as the separation improves. Underflow streams were found to be much more susceptible to hydrolysis than overflow streams, regardless of whether the hydrolysis was carried out right away or on dried samples, and also regardless of whether rinsing was applied. In flow system, dried underflow stream and commercialwheat starch were hydrolyzed using Orbamil-T ( Bacillus licheniformis ), Orbamil-BHT ( Bacillus stearothermophilus ), and Sigma f -amylase ( Bacillus licheniformis ). Hydrolysis of fresh starch was found to be significantly faster than commercial wheat starch. Commercial f -amylase Orbamil-T was found to be almost as effective as the purified Sigma f -amylase.     

Aflatoxin M1 in raw and ultra high temperature-treated milk commercialized in Portugal

During June to September 1999, 31 samples of raw milk were obtained from individual farms and 70 samples of ultrahigh-temperature-treated (UHT) milk (18 samples of whole milk, 22 of semi-skimmed and 30 samples of skimmed milk) were collected in supermarkets in Lisbon, Portugal. The total number of samples analysed was 101. The incidence of aflatoxin M₁ (AFM₁     

Identification of a new analogue of sildenafil added illegally to a functional food marketed for penile erectile dysfunction

A new analogue of sildenafil was discovered to have been added illegally to a functional food marketed for penile erectile dysfunction. The structure of the analogue was established by various NMR spectroscopic techniques (including DEPT, COSY, TOCSY, HMQC, HMBC). Because of the addition of a methylene group to sildenafil, the main ingredient of Viagra®, it was given the name homosildenafil, and this has never been reported previously. An analytical method using HPLC was proposed. Homosildenafil was added as a new inspection item and other foods have since been discovered to contain it.     

Survey for fumonisin B1 in Korean corn-based food products

Seventy-six corn-based foods collected in Seoul, Korea, including corn flakes, corn snack, cornstarch, corn for popping, roasted corn for tea, canned sweet corn and other corn products were analysed for the occurrence of fumonisin B₁ (FB₁) by using direct competitive enzyme-linked immunosorbent assay (dcELISA) and high-performance liquid chromatography (HPLC). The average recoveries of FB₁ from the corn flakes sample in the range 5-1000 ng g^-1 were 104% by dcELISA and 82% by HPLC. The limits of detection were approximately 5 ng g^-1 by dcELISA and 20 ng g^-1 by HPLC. The incidences and mean levels of FB₁ were 73.3, 78.6, 50, 58.3, 17.6 and 40% and 41.8, 67.9, 114, 256, 172 and 22 ng g^-1 from corn flakes, corn snack, corn starch, corn for popping, roasted corn for tea and other corn products, respectively, by dcELISA. No FB₁ was found in canned sweet corn. The results obtained by dcELISA were correlated to those by HPLC for FB₁ (r² = 0.992). This is the first report on the occurrence of FB₁ in corn-based foods in Korea.