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1.
J AOAC Int ; 98(3): 566-574, 2015.
Article in English | MEDLINE | ID: mdl-26025252

ABSTRACT

Florfenicol (FFC) residues in foods are regulated as the sum of florfenicol and its metabolites measured as florfenicol amine (FFA). An isotope dilution LC-MS/MS method utilizing phenylboronic acid (PBA) SPE cleanup is established for the accurate determination of FFA in fish muscles (i.e., salmon and tilapia) after acid catalyzed hydrolysis. Comparisons of the PBA SPE cleanup procedure with other cleanup procedures such as mixed-mode cationic (MCX) SPE and solid supported liquid-liquid extraction were performed. Quantification of FFA in fish muscles was accomplished by using matrix-matched calibration with FFA-D3 as the internal standard. The method was validated with FFA fortified fish muscles at three different levels (50, 100, and 200 µg/kg). Conversion of FFC to FFA by acid catalyzed hydrolysis was evaluated and found to be ≥88%. The recoveries of FFA in fish muscles at the three fortification levels ranged from 89 to 106%, and RSDs were ≤9% in all cases. The LOD values in salmon and tilapia muscles were 0.13 and 1.64 µg/kg, respectively. The LOQ values in salmon and tilapia muscles were 0.29 and 4.13 µg/kg, respectively. This method is suitable for the application in routine control of FFC in fishes according to its residue definition.


Subject(s)
Anti-Bacterial Agents/analysis , Boronic Acids/chemistry , Fishes/metabolism , Muscles/chemistry , Thiamphenicol/analogs & derivatives , Animals , Calibration , Chromatography, High Pressure Liquid , Drug Residues/analysis , Food Analysis , Limit of Detection , Radioisotope Dilution Technique , Reproducibility of Results , Solid Phase Extraction , Tandem Mass Spectrometry , Thiamphenicol/analysis
2.
Anal Bioanal Chem ; 407(11): 3009-21, 2015 Apr.
Article in English | MEDLINE | ID: mdl-25619984

ABSTRACT

This paper presents the certification of alpha-endosulfan, beta-endosulfan, and endosulfan sulfate in a candidate tea certified reference material (code: GLHK-11-03) according to the requirements of the ISO Guide 30 series. Certification of GLHK-11-03 was based on an analytical method purposely developed for the accurate measurement of the mass fraction of the target analytes in the material. An isotope dilution mass spectrometry (IDMS) method involving determination by (i) gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) and (ii) gas chromatography-electron ionization-high-resolution mass spectrometry (GC-EI-HRMS) techniques was employed. The performance of the described method was demonstrated through participation in the key comparison CCQM-K95 "Mid-Polarity Analytes in Food Matrix: Mid-Polarity Pesticides in Tea" organized by the Consultative Committee for Amount of Substance-Metrology in Chemistry in 2012, where the study material was the same as the certified reference material (CRM). The values reported by using the developed method were in good agreement with the key comparison reference value (KCRV) assigned for beta-endosulfan (727 ± 14 µg kg(-1)) and endosulfan sulfate (505 ± 11 µg kg(-1)), where the degree of equivalence (DoE) values were 0.41 and 0.40, respectively. The certified values of alpha-endosulfan, beta-endosulfan, and endosulfan sulfate in dry mass fraction in GLHK-11-03 were 350, 730, and 502 µg kg(-1), respectively, and the respective expanded uncertainties, due to sample inhomogeneity, long-term and short-term stability, and variability in the characterization procedure, were 27 µg kg(-1) (7.8 %), 48 µg kg(-1) (6.6 %), and 33 µg kg(-1) (6.6 %).


Subject(s)
Endosulfan/analogs & derivatives , Endosulfan/analysis , Gas Chromatography-Mass Spectrometry/standards , Pesticides/analysis , Tea/chemistry , Calibration , Chemical Fractionation , Endosulfan/standards , Food Analysis/methods , Food Analysis/standards , Gas Chromatography-Mass Spectrometry/methods , Hydrocarbons, Chlorinated/analysis , Isomerism , Pesticide Residues/analysis , Pesticides/standards , Radioisotope Dilution Technique , Reference Standards , Sensitivity and Specificity
3.
Anal Bioanal Chem ; 405(23): 7241-50, 2013 Sep.
Article in English | MEDLINE | ID: mdl-23831828

ABSTRACT

This paper describes a metrological approach to evaluate the measurement capability of laboratories participating in two proficiency testing (PT) programmes involving the analysis of five polycyclic aromatic hydrocarbons (PAHs) in sediment samples. Reference values of PAHs in the programmes for performance assessment were obtained from an accurate isotope dilution gas chromatography mass spectrometry (ID-GCMS) method which was thoroughly validated and verified. Isotope dilution mass spectrometry (IDMS) technique usually has a well-defined measurement uncertainty budget and a traceability link to an International System of Units. Provision of the metrological reference values in PT enables the establishment of a technical platform to assess the actual competence of the participating laboratories in sediment PAHs analysis. Results of the PT programmes showed that about 80 % of the laboratories employed gas chromatography in their analyses and the remaining used liquid chromatography. Irrespective of the techniques being used, however, the majority of the participating laboratories were observed to underestimate values in which the mean values of the five reported PAHs were less than those of the ID-GCMS-derived reference values by 13-20 %. Only 41-44 % of the participating laboratories were able to achieve satisfactory z-scores. The present study revealed that the reinforcement of the capability for accurate measurement of PAHs in sediment samples in laboratories worldwide should be addressed.

4.
Anal Chim Acta ; 721: 110-4, 2012 Apr 06.
Article in English | MEDLINE | ID: mdl-22405308

ABSTRACT

This paper presents the preparation of a candidate certified reference material (CRM) of cypermethrin in green tea, GLHK-11-01a according to the requirements of ISO Guide 34 and 35. Certification of the material was performed using a newly developed isotope dilution mass spectrometry (IDMS) approach, with gas chromatography high resolution mass spectrometry (GC-HRMS) and gas chromatography-tandem mass spectrometry (GC-MS/MS). Statistical analysis (one-way ANOVA) showed excellent agreement of the analytical data sets generated from the two mass spectrometric detections. The characterization methods have also been satisfactorily applied in an Asia-Pacific Metrology Program (APMP) interlaboratory comparison study. Both the GC-HRIDMS and GC-IDMS/MS methods proved to be sufficiently reliable and accurate for certification purpose. The certified value of cypermethrin in dry mass fraction was 148 µg kg(-1) and the associated expanded uncertainty was 14µg kg(-1). The uncertainty budget was evaluated from sample in homogeneity, long-term and short-term stability and variability in the characterization procedure. GLHK-11-01a is primarily developed to support the local and wider testing community on need basis in quality assurance work and in seeking accreditation.

5.
Forensic Sci Int ; 219(1-3): 272-7, 2012 Jun 10.
Article in English | MEDLINE | ID: mdl-22300796

ABSTRACT

This paper discusses the organization of the first international proficiency test (PT) programme on ketamine (K) and norketamine (NK) in hair samples. The primary objective of the programme was to evaluate the analytical capability of participating laboratories on hair analysis for K and NK via comparison of results. Authentic samples, instead of spiked samples were used in the programme to mimic the analysis of incorporated illicit drugs in real-life situations. Eight of the ten participating medical or forensic laboratories from Australia, France, Hong Kong, Italy, Singapore and the USA returned results to the organizer. Quantification methods from these laboratories were confined to GC-MS and LC-MS/MS. Performance assessment based on z-score indicated that only three laboratories achieved satisfactory results for both the analysis of K and NK. It was concluded that the overall performance of the participating laboratories was fair and there is still room for further improvement. Additional similarly designed PT programmes are recommended to be organized in order to encourage reliable measurements of illicit drugs in hair samples. Taking into account the substantial effect on the consensus values within limited number of data points, a recommendation on the provision of reference values assigned by accurate methods will be of benefit to small size PT programmes in the forensic field.


Subject(s)
Anesthetics, Dissociative/analysis , Hair/chemistry , Ketamine/analogs & derivatives , Ketamine/analysis , Laboratories/standards , Chromatography, Liquid , Forensic Toxicology/standards , Gas Chromatography-Mass Spectrometry , Humans , Internationality
6.
J Agric Food Chem ; 59(10): 5195-203, 2011 May 25.
Article in English | MEDLINE | ID: mdl-21491855

ABSTRACT

Abalones ( Haliotis species) are a popular delicacy and commonly preserved in dried form either whole or in slices or small pieces for consumption in Asian countries. Driven by the huge profit from trading abalones, dishonest traders may substitute other molluscan species for processed abalone, of which the morphological characteristics are frequently lost in the processed form. For protection of consumer rights and law enforcement against fraud, there is a need for an effective methodology to differentiate between fake and genuine abalone. This paper describes a method (validated according to the international forensic guidelines provided by SWGDAM) for the identification of fake abalone species using forensically informative nucleotide sequence (FINS) analysis. A study of the local market revealed that many claimed "abalone slice" samples on sale are not genuine. The fake abalone samples were found to be either volutids of the genus Cymbium (93%) or the muricid Concholepas concholepas (7%). This is the first report of Cymbium species being used for the preparation and sale as "abalone" in dried sliced form in Hong Kong.


Subject(s)
Gastropoda/classification , Gastropoda/genetics , Seafood/classification , Sequence Analysis, DNA/methods , Animals , Forensic Sciences/methods , Fraud/legislation & jurisprudence , Legislation, Food , RNA, Ribosomal, 16S/genetics
7.
J AOAC Int ; 90(4): 1133-41, 2007.
Article in English | MEDLINE | ID: mdl-17760352

ABSTRACT

An interlaboratory comparison study for the determination of 5 residual organochlorine pesticides (hexachlorobenzene and 4 hexachlorocyclohexane isomers) in ginseng root was performed. This program [Asia Pacific Laboratory Accreditation Cooperation (APLAC) T049] was the first of its kind for an herbal matrix and involved the participation of 70 laboratories from 26 countries worldwide. Consensus mean values were computed statistically from the reported results, which were eventually used to assess the performance of individual laboratories in terms of the z-scores. The distribution of analytical data was found to be widespread, with standard deviation ranging from 43.9 to 55.9%, and the result patterns obtained were similar to those residue pesticide programs using other matrixes. Although the estimation of measurement uncertainty is a crucial requirement for all quantitative tests for laboratories that meet the requirements of International Organization for Standardization/International Electrotechnical Commisssion (ISO/IEC) 17025, some laboratories in this program had difficulties and showed unfamiliarity with respect to that quality criterion. It was recommended that laboratories review and rectify the situation promptly so that they would have a better understanding of measurement uncertainty or the test service provided.


Subject(s)
Chromatography, Gas/methods , Food Analysis/methods , Food Contamination , Panax/metabolism , Pesticide Residues/analysis , Pesticides/analysis , Plant Roots/metabolism , Chlorine/analysis , Clinical Laboratory Techniques , Electrochemistry/methods , Hydrocarbons, Chlorinated/chemistry , Quality Control , Reproducibility of Results
8.
J Agric Food Chem ; 55(9): 3249-57, 2007 May 02.
Article in English | MEDLINE | ID: mdl-17407305

ABSTRACT

An international CCQM-P60 pilot study involving eight national metrological institutes was organized to investigate if the quantification of genetically modified (GM) corn powder by real-time PCR was affected by the DNA extraction method applied. Four commonly used extraction methods were compared for the extraction of DNA from a GM Bt176 corn powder. The CTAB-based method yielded the highest DNA template quantity and quality. A difference in the 260 nm/230 nm absorbance ratio was observed among the different extraction methods. Real-time amplification of sequences specific for endogenous genes zein and hmg as well as transgenic sequences within the cryIA(b) gene and a fragment covering the junction between the transformed DNA and the plant genome were used to determine the GM percentage. The detection of the transgenic gene was affected by the quantity and quality of template used for the PCR reaction. The Bt176 percentages measured on diluted or purified templates were statistically different depending on the extraction method applied.


Subject(s)
Bacterial Proteins/genetics , Bacterial Toxins/genetics , DNA, Plant/isolation & purification , Endotoxins/genetics , Food, Genetically Modified , Hemolysin Proteins/genetics , Plants, Genetically Modified/genetics , Polymerase Chain Reaction/methods , Zea mays/genetics , Bacillus thuringiensis Toxins , DNA, Plant/analysis , Seeds/genetics
9.
J Agric Food Chem ; 55(9): 3339-45, 2007 May 02.
Article in English | MEDLINE | ID: mdl-17407316

ABSTRACT

A highly accurate and precise method based on isotope dilution gas chromatography-mass spectrometry was developed for the determination of five matrix-bound organochlorine pesticides, namely, hexachlorobenzene and hexachlorocyclohexanes (alpha-, beta-, delta-, and gamma- isomers), in a reference sample of Panax gingseng. Identification of the analytes was confirmed under selective ion monitoring mode by the presence of two dominant ion fragments within the specific time windows (+/-1% of the relative retention time with respect to the calibration standards) and matching of relative ion intensities of the concerned ions in samples and calibration standards (within +/-5%). Quantification was based on the measurement of concentration ratios of the natural and isotopic analogues in the sample and calibration blends. To circumvent the tedious iterative process of exact isotope matching that is often used in isotope dilution mass spectrometry analysis, a single-point calibration procedure was adopted with the isotopic amount ratios in the sample and calibration blends close to unity (0.9-1.1). Under the described approach, intraday and interday repeatability of replicate analyses of organochlorine pesticides in the ginseng root sample were below 1.4%. The expanded relative uncertainty ranging from 4.0 to 6.5% at a coverage factor of 2 was significantly lower than those of conventional gas chromatographic methods using other calibration techniques (internal or external standards). A deviation of less than 2.0% from the certified values was achieved when applying the developed method to determine hexachlorobenzene, alpha-, and beta-hexachlorocyclohexane in a certified reference material (CRM), BCR-CRM 115. Because of the unavailability of relevant CRMs of herbal origins, the concerned ginseng root sample, after verification of the "true values" of the concerned organochlorine pesticides by the valid primary method, is suitable for serving as an in-house reference material for quality assurance and method validation purposes.


Subject(s)
Gas Chromatography-Mass Spectrometry/methods , Hydrocarbons, Chlorinated/analysis , Indicator Dilution Techniques , Panax/chemistry , Pesticide Residues/analysis , Plant Roots/chemistry , Carbon Isotopes
10.
J Agric Food Chem ; 54(19): 7159-66, 2006 Sep 20.
Article in English | MEDLINE | ID: mdl-16968077

ABSTRACT

Seeds of melon (Citrullus lanatus var. sp.), pumpkin (Cucurbita moschata), and sunflower (Heliantus annus) were gamma-irradiated at 1, 3, 5, and 10 kGy and analyzed by electron paramagnetic resonance (EPR) and gas chromatography-mass spectrometry (GC-MS) according to EN1787:2000 and EN1785:2003, respectively. Distinguishable triplet signals due to the presence of induced cellulose radicals were found at 2.0010-2.0047 g in the EPR spectra. The gamma-irradiated radiolytic markers of 2-dodecylcyclobutanone (2-DCB) and 2-tetradecylcyclobutanone (2-TCB) were identified in all irradiated seed samples. Both the free radicals and the alkylcyclobutanones were found to increase with irradiation dose. In general, linear relationships between the amount of radicals and irradiation dosage could be established. Studies at an ambient temperature (20-25 degrees C) in a humidity-controlled environment showed a complete disappearance of the cellulosic peaks for irradiated samples upon 60 days of storage. Such instability behavior was considered to render the usefulness of using EPR alone in the determination of irradiated seed samples. On the other hand, 2-DCB and 2-TCB were also found to decompose rapidly (>85% loss after 120 days of storage), but the radiolytic markers remained quantifiable after 120 days of postirradiation storage. These results suggest that GC-MS is a versatile and complimentary technique for the confirmation of irradiation treatment to seeds.


Subject(s)
Cucurbita/radiation effects , Cucurbitaceae/radiation effects , Food Irradiation , Gas Chromatography-Mass Spectrometry , Helianthus/radiation effects , Seeds/radiation effects , Cucurbita/chemistry , Cucurbitaceae/chemistry , Electron Spin Resonance Spectroscopy , Gamma Rays , Seeds/chemistry
11.
Anal Bioanal Chem ; 385(1): 181-8, 2006 May.
Article in English | MEDLINE | ID: mdl-16547744

ABSTRACT

Liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-MS/MS) was applied to the determination of residual bacitracin A, colistin A, and colistin B in milk and animal tissue samples. Prior to instrumental analysis, samples were subjected to acid extraction followed by solid-phase cleanup using Strata-X cartridges. Mass spectral acquisitions were performed under selective multiple reaction monitoring (MRM) mode at m/z 199 and 670 from triply charged precursors of bacitracin A (m/z 475); m/z 385 and 379 from triply charged precursors of colistin A (m/z 391); and m/z 380 and 374 from triply charged precursors of colistin B (m/z 386). Method precision was evaluated from spike recovery of samples fortified at concentrations corresponding to 2/5 of the maximum residue limits (MRLs) for each of the analytes under study. Intra-day and inter-day variations were found to range from 90.9 to 104% with relative standard deviation (RSD) <6.5%, and from 90.1 to 106% with RSD <9.1%, respectively. Limits of quantification (LOQs) were defined as the spiking concentrations at 2/5 MRL, and limits of detection (LODs) were 10-47 microg kg(-1) for bacitracin A, 1-16 microg kg(-1) for colistin A, and 6-14 microg kg(-1) for colistin B in milk and animal tissues. The presented method has good precision and high sensitivity and was applied as a fast screening protocol and a quantitative tool for monitoring of the concerned polypeptides in foods as part of a surveillance program.


Subject(s)
Bacitracin/analysis , Chromatography, Liquid/methods , Colistin/analysis , Drug Residues/analysis , Milk/chemistry , Tandem Mass Spectrometry/methods , Animals , Cattle , Liver/chemistry , Molecular Structure , Muscle, Skeletal/chemistry , Poultry , Swine
12.
J AOAC Int ; 89(6): 1496-514, 2006.
Article in English | MEDLINE | ID: mdl-17225594

ABSTRACT

A study of single-laboratory validation (SLV) of a reversed-phase liquid chromatography (RP-LC) method was conducted for the determination of diester-diterpene Aconitum alkaloids, viz., aconitine, mesaconitine, and hypaconitine, in a variety of dietary supplements, including single- and multiple-ingredient dry powder extracts, pills, capsules, and raw materials. The Aconitum alkaloids in the samples were extracted by diethyl ether in the presence of ammonia. After cleanup with solid-phase extraction to remove the matrix interferences, the alkaloids were determined by RP-LC with UV detection at 235 nm, and the results were confirmed by tandem mass spectrometry. The linear responses for aconitine, mesaconitine, and hypaconitine based on the present LC system ranged from 0.5 to 200 microg/mL. Relative standard deviations of 2.0 to 6.9% were obtained from duplicate analysis of 6 test materials of different matrixes for the 3 Aconitum alkaloids performed by 2 analysts on 5 different days. The recoveries determined for supplements and raw materials spiked with 3 Aconitum alkaloids at levels of 2.5-10 microg/g were in the range of 86-99%. In view of the attainment of satisfactory results for accuracy, precision, and recovery in the SLV study, it is recommended that the method validation process proceed to a collaborative study.


Subject(s)
Aconitum/chemistry , Alkaloids/analysis , Dietary Supplements/analysis , Calibration , Capsules , Chromatography, High Pressure Liquid , Indicators and Reagents , Mass Spectrometry , Plant Extracts/analysis , Reference Standards , Reproducibility of Results , Spectrophotometry, Ultraviolet , Tablets
13.
Environ Pollut ; 137(2): 334-44, 2005 Sep.
Article in English | MEDLINE | ID: mdl-15963372

ABSTRACT

Samples from Hong Kong, China, were analyzed for organic carbon (OC), elemental carbon (EC), and total carbon (TC) by three thermal protocols (low-temperature IMPROVE and high-temperature STN and NIOSH) and two optical monitoring methods: reflectance and transmittance. Good agreement (+/-10%) for TC among the three protocols was observed for sample loadings of 1-55 microg m(-3). The two protocols using a reflectance pyrolysis correction showed best agreement for EC, with <20% differences found for approximately 80% of the samples. Hong Kong has a large diesel fleet, and for some heavily loaded samples the light transmittance was too low for quantitative detection, resulting in large uncertainties in the OC/EC split based on transmittance. Hong Kong experienced OC levels similar to those at US sites, but has much higher EC concentrations. OC/EC ratios range from 2 to 5 at two US sites and from 0.2 to 1.2 at three Hong Kong sites.


Subject(s)
Air Pollutants/analysis , Carbon/analysis , Environmental Monitoring/methods , Vehicle Emissions , Aerosols , Hong Kong , Optics and Photonics , Particle Size , Sensitivity and Specificity
14.
J Air Waste Manag Assoc ; 55(3): 291-301, 2005 Mar.
Article in English | MEDLINE | ID: mdl-15828671

ABSTRACT

The results of a 12-month study of more than 100 solvent extractable organic compounds (SEOC) in particulate matter (PM) less than or equal to 2.5 microm (PM2.5) collected at three air monitoring stations located at roadside, urban, and rural sites in Hong Kong are reported. The total yield of SEOC that accounts for approximately 8-18% of organic carbon (OC) determined by a thermal optical transmittance method was 125-2060 ng/m3, which included 14.6-128 ng/m3 resolved aliphatic hydrocarbons, 39.4-1380 ng/m3 unresolved complex mixtures, 0.6-17.2 ng/m3 polycyclic aromatic hydrocarbons, 41.6-520 ng/m3 fatty acids, and < 0.1-12.1 ng/m3 alkanols. Distinct seasonal variations (summer/winter differences) were observed with higher concentrations of the total and each class of SEOC in the winter and lower concentrations in the summer. Spatial variations are also obvious, with the roadside samples having the highest concentrations of SEOC and the rural samples having the lowest concentrations in all seasons. Characteristic ratios of petroleum hydrocarbons, such as carbon preference index, unresolved to resolved components, and carbon number with maximum concentration, suggest that PM2.5 carbon in Hong Kong originates from both biogenic and anthropogenic sources. The proportion of SEOC in PM2.5 from anthropogenic sources is estimated.


Subject(s)
Air Pollutants/analysis , Organic Chemicals/analysis , Air Pollutants/isolation & purification , Environmental Monitoring , Hong Kong , Organic Chemicals/isolation & purification , Particle Size , Seasons , Solvents
15.
Sci Total Environ ; 338(3): 267-81, 2005 Feb 15.
Article in English | MEDLINE | ID: mdl-15713334

ABSTRACT

Chemically speciated PM2.5 measurements were made at roadside, urban, and rural background sites in Hong Kong for 1 year during 2000/2001 to determine the spatial and temporal variations of PM2.5 mass and chemical composition in this highly populated region. Annual average PM2.5 concentrations at the urban and rural sites were 34.1 and 23.7 microg m(-3), respectively, approximately 50-100% higher than the United States' annual average National Ambient Air Quality Standard (NAAQS) of 15 microg m(-3). Daily PM2.5 concentrations exceeded the U.S. 24-h NAAQS of 65 microg m(-3) on 19 days, reaching 131+/-8 microg m(-3) at the roadside site on 02/28/2001. Carbonaceous aerosol is the largest contributor to PM2.5 mass (explaining 52-75% of PM2.5 mass at the two urban sites and 32% at the background site), followed by ammonium sulfate (ranging from 23% to 37% at the two urban sites and 51% at the background site). Ammonium sulfate and crustal concentrations showed more uniform spatial distributions, while the largest urban-rural contrasts found in carbonaceous aerosol (likely due to emissions from on-road gasoline and diesel vehicles). Marine influences accounted for 7% of the mass at the background site (more than twice as much as at the two urban sites). Ternary diagrams are utilized to illustrate the different spatial patterns.

16.
J Pharm Biomed Anal ; 34(3): 651-9, 2004 Feb 18.
Article in English | MEDLINE | ID: mdl-15127821

ABSTRACT

A sensitive method for determining lincomycin in bovine milk, animal muscles and organs using liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) is presented. Milk and homogenized animal tissues were extracted with acetonitrile twice after addition of an appropriate amount of clindamycin, a lincosamide analogue as the internal standard. The combined extracts were finally made up to 10 ml with distilled water and partitioned with hexane to remove the animal fats prior to analysis. Analytes in the extracts were separated on a reversed phase C18 column (250 mm x 2.1 mm, 5 microm) using a mobile phase of a 3:7 (v/v) mixture of 0.1% formic acid in acetonitrile and an ammonium formate buffer (ammonium formate:formic acid:acetonitrile:water, 1:5:50:950, v/v/v/v) running at a flow rate of 0.2 ml min(-1). Presence of lincomycin was confirmed by the presence of two characteristic product ions at m/z 126.1 and 359.2 within a defined retention time window from the precursor ion at m/z 407.2, whilst quantification was based on the relative ratio of the sum of the peak areas at m/z 126.1 and 359.2 for lincomycin to that of the internal standard (peaks at m/z 126.1 and 377.2) with reference to the respective ratios of the calibration standards. The validated method that was found to have linear responses in the calibration range from 25 to 3000 microg kg(-1) and satisfactory intra-day and inter-day accuracy (94.4-107.8%) and precision (1.3-7.8%) at concentrations ranging from 100 to 1500 microg kg(-1) has been applied to real samples and matrix spiked samples. It is considered robust and suitable for analysis of lincomycin in milk and animal tissues.


Subject(s)
Lincomycin/analysis , Milk/chemistry , Spectrometry, Mass, Electrospray Ionization/methods , Animals , Cattle , Chickens , Chromatography, Liquid/methods , Drug Evaluation, Preclinical/methods , Female , Lincomycin/chemistry , Lincomycin/metabolism , Milk/metabolism , Swine , Tissue Distribution/physiology
17.
J Chromatogr A ; 1061(2): 123-31, 2004 Dec 24.
Article in English | MEDLINE | ID: mdl-15641354

ABSTRACT

A simple, cost-effective, and high throughput method using on-line column-switching liquid chromatography fluorescence detection was developed and validated for analysing five (fluoro)quinolones (FQs)--enrofloxacin (ENRO), ciprofloxacin (CIPR), sarafloxacin (SARA), oxolinic acid (OXOL), and flumequine (FLUM) in bovine milk. Norfloxacin (NORF) and nalixidic acid (NALI) were used as internal standards. After simple deproteination of milk sample with 5% (w/v) metaphosphoric acid, the supernatant was subject to on-line column clean-up and direct analysis by LC-FLD. The extraction cartridge was prepared in-house by slurry packing with hydrophilic-lipophilic polymer sorbent. The accuracy of measurement for each (fluoro)quinolone at different maximum residue limits (MRL) was 101-103% (ENRO), 92.8-97.4% (CIPR), 89.8-92.8% (SARA), 116-121% (OXOL), and 81.3-85.5% (FLUM), whilst the precision was 2.9-6.1% (ENRO), 2.5-5.1% (CIPR), 2.3-5.0% (SARA), 3.1-5.9% (OXOL), and 5.6-6.5% (FLUM). The decision limits, detection capabilities, specificity and analytes stability during storage were also investigated.


Subject(s)
Anti-Bacterial Agents/analysis , Chromatography, Liquid/methods , Fluoroquinolones/analysis , Milk/chemistry , Spectrometry, Fluorescence/methods , Animals , Cattle , Chromatography, Liquid/instrumentation , Sensitivity and Specificity
18.
Chemosphere ; 52(9): 1397-403, 2003 Sep.
Article in English | MEDLINE | ID: mdl-12867169

ABSTRACT

Air samples were collected for characterisation of PCDD/Fs and other persistent organic pollutants (POPs) such as aldrin, alpha-HCH, beta-HCH, delta-HCH, gamma-HCH, o,p'-DDT, p,p'-DDT, o,p'-DDE, p,p'-DDE, o,p'-DDD, p,p'-DDD, dieldrin, endrin, endosulfan I and II, heptachlor, heptachlor epoxide and hexachlorobenzene during the winter of 2000/2001 at the weather station of the Hong Kong Observatory at Tai Mo Shan (TMS), which is the highest point (approximately 957 m) in Hong Kong, besides the routine monitoring of PCDD/Fs and 200 other toxic air pollutants (TAPs) at two urban TAPs stations at Tsuen Wan and Central & Western. Concentrations of the pollutants detected at TMS station were evaluated and compared to those recorded at the urban stations. Though pesticides including alpha-HCH, hexachlorobenzene, DDT, DDE, heptachlor, and endosulfan I were detected, these pesticides were found at relatively low concentrations of about 0.02-0.23 ng/m3 and should not have any significant health effects. Concentrations of some of the monitored POPs were found to be higher whilst most of the monitored TAPs were at comparable levels to those measured at the urban stations during the same period. According to the Stockholm Convention on POPs (May 2001), the 12 chemicals labelled by the United Nations as the most dangerous are: aldrin, chlordane, DDT, dieldrin, endrin, heptachlor, mirex, toxaphene, hexachlorobenzene, PCBs and dibenzo-p-dioxins/dibenzofurans (PCDDs)/(PCDFs). Given that there has not been any large scale use of organo-chlorine pesticides recorded since the decline of local farming activities in recent years, the results of the present study again show that pesticides and POPs such as PCDDs/PCDFs are ubiquitous environmental contaminants present in the atmosphere of Hong Kong. The findings also indicate that organo-chlorine pesticides and PCDDs/PCDFs are among the most prevalent chlorinated semi-volatile pollutants present in Hong Kong. Results obtained in the present study suggest that selected pesticides may be used as tracers for transport of pollutants for regional air quality study.


Subject(s)
Air Pollutants/analysis , Benzofurans/analysis , Benzofurans/chemistry , Environmental Monitoring , Hong Kong , Hydrocarbons, Chlorinated , Insecticides/analysis , Insecticides/chemistry , Meteorological Concepts , Seasons
19.
J Environ Monit ; 5(6): 989-96, 2003 Dec.
Article in English | MEDLINE | ID: mdl-14710944

ABSTRACT

This paper reports the monitoring results of eleven polycyclic aromatic hydrocarbons (PAHs), four to six-ring, at two urban sites-Central & Western (CW) and Tsuen Wan (TW) in Hong Kong from January to December 2000; and the findings of a study conducted in 2001 of the partitioning of the gaseous and particulate phases of PAHs. The sum of the eleven PAHs under study (sigmaPAHs) was found to range from 6.46 to 38.8 ng m(-3). The annual mean levels at 12.2 ng m(-3) and 15.8 ng m(-3) for CW and TW respectively are comparable to those recorded for the previous two years and are also within the reported ranges for other metropolitan cities in the Asia Pacific region. Amongst the selected eleven PAHs, fluoranthene and pyrene were the two most abundant found in the urban atmosphere of Hong Kong during the study period accounting for approximately 80%, of the total PAHs. The ratios of benzo(a)pyrene to benzo(g,h,i)perylene (BaP/BghiP) and indeno(1,2,3-cd)pyrene to benzo(g,h,i)perylene (IDP/BghiP) indicate that diesel and gasoline vehicular exhausts were the predominant local emission sources of PAHs. Seasonal variations with high winter to summer ratios for each of the individual PAHs (CW: 1.6-16.7 and TW: 0.82-8.2) and for sigmaPAHs (CW: 1.9 and TW: 1.8) and a spatial variation of BaP amongst the air monitoring stations are noted. Results of correlation studies illustrate that local meteorological conditions such as ambient temperature, solar radiation, wind speed and wind direction have significant impact on the concentrations of atmospheric PAHs accounting for the observed seasonal variations. A snapshot comparison of the concentrations of PAHs at four sites including a roadside site, a rural site and the two regular urban sites CW and TW was also performed using the profiles of PAHs recorded on two particulate episode days in March 2000.


Subject(s)
Air Pollutants/analysis , Polycyclic Aromatic Hydrocarbons/analysis , Environmental Monitoring , Hong Kong , Meteorological Concepts , Seasons
20.
Chemosphere ; 47(6): 647-53, 2002 May.
Article in English | MEDLINE | ID: mdl-12047076

ABSTRACT

A total of 27 ambient air samples of were collected from six locations in Hong kong during the period of January-August, 2000 and analysed for polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs). In all sampling locations, higher concentrations of PCDDs/PCDFs, ranging from 0.03 to 0.43 pg I-TEQ/m3 were measured in winter months (January and March) than in the summer months (July and August) of concentrations at 0.018-0.025 pg I-TEQ/m3. These concentrations are similar to annual ranges reported earlier for two Hong Kong urban sites and other urban cities in Asia. Europe, and the United States. Despite significant seasonal variations in ambient air concentrations of PCDD/Fs (expressed in I-TEQ) were observed, the congener profiles of all the samples in this study period were similar, with OCDD, 1,2,3,4,6,7,8-HpCDD, OCDF and 1,2,3,4,6,7,8-HpCDF being the predominant species. However, the homologue profiles for the samples collected at the six locations of this study were found to display significantly different spatial and seasonal trends.


Subject(s)
Air Pollutants/analysis , Benzofurans/analysis , Polychlorinated Dibenzodioxins/analogs & derivatives , Polychlorinated Dibenzodioxins/analysis , Soil Pollutants/analysis , Dibenzofurans, Polychlorinated , Environmental Monitoring , Hong Kong , Seasons
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