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浙江大学学报（医学版） 2012年第1期41卷 19-24页

作者：程玲徐毅敏季申冷晶毛秀红王柯王书芳浙江大学药学院浙江杭州310058 上海市食品药品检验所上海201203

目的:建立同时测定白芍中有机氯、有机磷和拟除虫菊酯类等15种农药残留的大体积进样-气相色谱-质谱联用(LVI-GC-MS)分析方法。方法:采用大体积进样-气相色谱-质谱法,色谱柱为DB-5MS毛细管柱(30 m×250μm,0.25μm),程序升温:初始温... 详细信息

目的:建立同时测定白芍中有机氯、有机磷和拟除虫菊酯类等15种农药残留的大体积进样-气相色谱-质谱联用(LVI-GC-MS)分析方法。方法:采用大体积进样-气相色谱-质谱法,色谱柱为DB-5MS毛细管柱(30 m×250μm,0.25μm),程序升温:初始温度40℃保持1 min,然后以20℃/min升至210℃保持2 min,以5℃/min升至280℃保持22 min。进样量15μl,流速1.0 ml/min。结果:各农药在一定质量浓度范围内线性关系良好,相关系数r=0.9937～0.9995。在10μg/kg和100μg/kg两个质量浓度水平下,各农药的回收率为60.4%～106.8%(除二甲戊乐灵和4,4'-DDE为53.1%、45.2%外),相对标准偏差(RSD)为3.6%～18.6%,检测限(S/N=3)为0.16～3.59μg/kg。样品中检测到4,4'-DDE,其含量远低于药典规定的残留限量。结论:本研究建立的LVI-GC-MS方法操作简单、准确、灵敏度高、成本低,可以实现白芍药材中多农药残留的快速检测。

关键词：白芍/分析气相色谱-质谱法农药残留量/分析杀虫药有机氯/分析有机磷化合物/分析除虫菊酯类/分析

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Multiresidue method for determination of sulfonylurea herbicides in water by liquid chromatography with confirmation by capillary electrophoresis

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JOURNAL OF AOAC INTERNATIONAL 1999年第6期82卷 1523-1533页

作者： Hickes, H Watrous, M Montana State Univ Agr Sci Div Lab Bur Montana Dept Agr Bozeman MT 59717 USA

A liquid chromatographic method with comfirmation by capillary electrophoresis was used to determine 12 sulfonylurea herbicides in agricultural water. Analysis of 3 different water matrixes fortified at 2 levels gave good recoveries with adequate sensitivity at the 0.1 ppb level. A portion of the water was acidified with acetic acid and loaded onto an RP-102 solid-phase extraction (SPE) cartridge, and the extract was cleaned up on an alumina SPE cartridge. Extracts were desalted with an RP-102 SPE cartridge before instrumentation. Samples needing chemical filtration, such as pond water, required additional cleanup with a SAX SPE cartridge before the alumina cleanup step. Data were compiled for both determinative techniques and evaluated.

关键词：醋酸色谱法液相/方法电泳毛细管除莠剂/分析氢离子浓度农药残留量/分析敏感性与特异性磺酰脲化合物/分析水/化学

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Determination of regularly distributed plant protectants in raw and drinking waters, using a multiresidue method with cyclodextrin-modified micellar electrokinetic chromatography

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JOURNAL OF AOAC INTERNATIONAL 1999年第6期82卷 1510-1522页

作者： Stutz, H Malissa, H Salzburg Univ Inst Chem & Biochem A-5020 Salzburg Austria

Eighteen plant protectant compounds were separated and determined by cyclodextrin-modified micellar electrokinetic chromatography (MEKC) in a multiclass/multiresidue method. The pesticides included are those dispersed in the greatest amounts today over agricultural acreage, and they represent 8 different classes of compounds (azoles, benzoic acids, chloroacetanilides, phenoxy acids, phenylureas, sulfonylureas, thiocarbamates, and triazines) covering a wide range of chemical reactivities and physicochemical properties. A 500 mt sample of tap water is preconcentrated by solid-phase extraction (SPE) with 300 mg combined polystyrene-divinylbenzene and methacrylate macroporous resins. Trapped analytes are eluted collectively with diethyl ether. Concentration and solvent change yield 250 mu L of an acetone "concentrate," which is further worked up and concentrated 1:10 to produce the MEKC injection solution containing 10 mmol/L sodium dodecyl sulfate (SDS) surfactant, For MEKC, 2 phosphate/SDS buffer systems were designed, each allowing complete separation of all pesticides in a single run. Sensitivity was enhanced by a self-etched bubble cell and an injection procedure which employs stacking at reversed polarity. The ability of MEKC to determine plant protectants in raw and drinking waters at the 0.1 mu g/L level, as demanded by the guidelines of the European Union, was demonstrated with spiked tap waters. Recoveries were between 75 and 110%, and limits of quantification, evaluated as method detection limits according to guidelines of the U.S. Environmental Protection Agency, ranged between 0.03 and 0.10 mu g/L. The precisions of the relative migration times were all below 0.5%.

关键词：醋酸缓冲剂色谱法胶束电动毛细管/方法环糊精类氢离子浓度农药残留量/分析质量控制水/化学

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A fully automated system for analysis of pesticides in water: On-line extraction followed by liquid chromatography tandem photodiode array/postcolumn derivatization/fluorescence detection

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JOURNAL OF AOAC INTERNATIONAL 1999年第4期82卷 968-981页

作者： Patsias, J Papadopoulou-Mourkidou, E Aristotle Univ Thessaloniki Pesticide Sci Lab GR-54006 Thessaloniki Greece

A fully automated system for on-line solid phase extraction (SPE) followed by high-performance liquid chromatography (HPLC) with tandem detection with a photodiode array detector and a fluorescence detector (after postcolumn derivatization) was developed for analysis of many chemical classes of pesticides and their major conversion products in aquatic systems. An automated on-line-SPE system (Prospekt) operated with reversed-phase cartridges (PRP-1) extracts analytes from 100 mL acidified (pH = 3) filtered water sample. On-line HPLC analysis is performed with a 15 cm C-18 analytical column eluted with a mobile phase of phosphate (pH = 3)-acetonitrile in 25 min linear gradient mode. Solutes are detected by tandem diode array/derivatization/fluorescence detection. The system is controlled and monitored by a single computer operated with Millenium software. Recoveries of most analytes in samples fortified at 1 mu g/L are >90%, with relative standard deviation values of <5%. For a few very polar analytes, mostly N-methylcarbamoyloximes (i.e., aldicarb sulfone, methomyl, and oxamyl), recoveries are <20%. However, for these compounds, as well as for the rest of the N-methylcarbamates except for aldicarb sulfoxide and butoxycarboxim, the limits of detection (LODs) are 0.005-0.05 mu g/L. LODs for aldicarb sulfoxide and butoxycarboxim are 0.2 and 0.1 mu g, respectively. LODs for the rest of the analytes except 4-nitrophenol, bentazone, captan, decamethrin, and MCPA are 0.05-0.1 mu g/L. LODs for the latter compounds are 0.2-1.0 mu g/L. The system can be operated unattended.

关键词：自动分析氨甲酸酯类色谱法高压液相/方法气相色谱-质谱法/方法希腊除莠剂/分析杀虫药/分析农药残留量/分析敏感性与特异性水/化学

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Analysis of pesticide residues in fruits, vegetables, and milk by gas chromatography/tandem mass spectrometry

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JOURNAL OF AOAC INTERNATIONAL 1999年第4期82卷 982-990页

作者： Sheridan, RS Meola, JR New York State Dept Agr & Markets Food Lab Albany NY 12235 USA

A method for detection, quantitation, and confirmation of more than 100 pesticides by gas chromatography (GC) with ion trap mass spectrometry (MS/MS) has been developed. The sensitivity of this method for many analytes is equal to or lower than those of selective GC detectors such as flame photometric detectors and electrolytic conductivity detectors. Using MS/MS, very low detection limits and good confirmation (1 precursor ion and 2 or more product ions) are achieved simultaneously. The entire list of pesticides is screened with 2 injections per sample. Samples are introduced onto the column by a temperature-programmed cold injection to maximize response. Each pesticide is run with its own unique set of parameters, which fragment the compound, retaining only the precursor ion. This ion is then refragmented to create a product spectrum. The selectivity of MS/MS gives a very clean spectrum, making compound identification and confirmation clear, even with a relatively dirty food matrix. If care is taken to maintain the injection port and guard column, this method can reliably identify and confirm more than 100 pesticides at the low parts-per-billion range.

关键词：食品污染水果/化学气相色谱-质谱法/方法乳/化学农药残留量/分析敏感性与特异性蔬菜/化学动物

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Pesticide residues in selected food commodities: Results from the Danish National Pesticide Monitoring Program 1995-1996

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JOURNAL OF AOAC INTERNATIONAL 1999年第2期82卷 337-358页

作者： Juhler, RK Lauridsen, MG Christensen, MR Hilbert, G Danish Vet & Food Adm Inst Food Res & Nutr DK-2860 Soborg Denmark

The paper presents results of analyses of 4182 samples collected from January 1995 to December 1996 for the Danish National Pesticide Monitoring Pro gram. The program basis is a random sample control supplemented with a target control. The objectives of the control are to monitor consumer exposure to health hazards and to enforce national and European Community regulations. The Danish Veterinary and Food Administration is responsible for establishing methods, data manipulation, and evaluation, but actual analyses are performed at 4 regional laboratories, In addition to a description of the Danish National Pesticide Monitoring Program on food, the effects of lowering the reporting limits are discussed. Pesticides included are those in current use as well as chlorinated pesticides like lindane, DDT, and HCB, occurring in food now primarily as a result of environmental contamination, Commodities analyzed are fruits, vegetables, cereals, bran, fish, and animal products such as meat, butter, cheese, fat, and eggs. In fruits and vegetables, residues were detected in 10% of 2515 samples, with higher incidences of detection for foreign commodities. Violation rate was 0.6%. In food of animal origin, low levels of organochlorine pesticides were detected in most fish samples and in more than half of the animal product samples. However, no results exceeding maximum residue limits were found. No residues of organcophosphorus pesticides were detected in the 231 meat samples analyzed.

关键词：乳制品/分析丹麦环境暴露环境监测鱼类食品分析/方法水果/化学杀真菌剂工业/分析烃类氯化杀虫药/分析肉/分析有机磷化合物农药残留量/分析蔬菜/化学动物

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Dietary intake and residues of organochlorine pesticides in foods from Hsinchu, Taiwan

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JOURNAL OF AOAC INTERNATIONAL 1999年第3期82卷 677-682页

作者： Doong, RA Lee, CY Sun, YC Natl Tsing Hua Univ Dept Nucl Sci Hsinchu 30043 Taiwan Natl Tsing Hua Univ Nucl Sci & Technol Dev Ctr Hsinchu 30043 Taiwan

The levels of contamination with various organochlorine pesticides (such as total HCH, heptachlor, heptachlor epoxide, aldrin, dieldrin, endrin, endosulfan, and total DDT) of different foods from 3 traditional markets were determined to estimate Taiwanese daily intake of organochlorine pesticides. Of the 18 organochlorine pesticides investigated, alpha-HCH, beta-HCH, lindane, delta-HCH, heptachlor, heptachlor epoxide, dieldrin, endrin, alpha-endosulfan, p,p'-DDE, and p,p'-DDT were detected at concentrations ranging from 0.26 to 10.2 ng/g wet weight. Contamination with organochlorine pesticides followed the order heptachlor > dieldrin > alpha-endosulfan > HCH isomers > heptachlor epoxide > DDT. Frequencies of detection of organochlorine pesticide residues ranged from 2.0 to 52.3%. alpha-Endosulfan was the most frequently detected organochlorine pesticide in the foods analyzed, followed by heptachlor epoxide (47.6%) and alpha-HCH (38.9%). Estimated daily intakes (EDIs) of organochlorine pesticides from foods were 1.137 mu g for total HCH, 2.147 mu g for heptachlor, 0.702 mu g for heptachlor epoxide, 0.624 mu g for endosulfan, 0.098 mu g for cyclodiene, and 0.541 mu g for total DDT These EDls were only 0.075% of the acceptable daily intake (ADI) for lindane, 47.5% of ADI for heptachlor and heptachlor epoxide, 0.045% of ADI for total DDT, and 1.01% of ADI for aldrin and dieldrin, Therefore, consumption of the foods analyzed does not pose a risk to consumer health.

关键词：色谱法气相膳食硫丹/分析食品分析食品污染七氯/分析杀虫药/投药和剂量杀虫药/分析肉/分析农药残留量/分析质量控制危险因素海味/分析台湾人类

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The impact of household preparations on the residues of pesticides in selected agricultural food commodities available in India

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JOURNAL OF AOAC INTERNATIONAL 1999年第3期82卷 725-737页

作者： Ramesh, A Balasubramanian, M Fredrick Inst Plant Protect & Toxicol Dept Pesticide Chem Chennai 601301 Tamil Nadu India

Gas chromatographic multiresidue methods for simultaneous determination of organophosphorus, organochlorine, and organonitrogen pesticides were used to study the exposure of the Indian population to pesticide contamination at their actual dietary intakes. Selected agricultural commodities-5 kinds of vegetables (tomato, potato, okra, cabbage, and green beans), 6 kinds of cereals and purses (rice, maize, wheat, red gram, black gram, and green gram), and 6 kinds of fruits (mango, orange, guava, banana, apple, and grapes)-readily available in Chennai City local markets-were studied for this purpose. Samples were fortified with known concentrations of various pesticides and subjected to household preparation methods commonly used in India. The impact of household preparation is very high, resulting in 65-95% decontamination of pesticides at different stages. Of 512 raw market samples analyzed, the organochlorine and organophosphorus pesticides present in 12 samples were removed during household preparations, resulting in residues well below the toxicologically acceptable limits.

关键词：色谱法气相净化食品分析食品污染食品处理和加工水果/化学烃类氯化印度杀虫药/分析最高容许浓度有机磷化合物农药残留量/分析蔬菜/化学人类

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POLYCHLORINATED BIPHENYLS, DIELDRIN AND DDT IN LAKE TROUT COOKED BY BROILING, ROASTING OR MICROWAVE

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BULLETIN OF ENVIRONMENTAL CONTAMINATION AND TOXICOLOGY 1979年第1-2期21卷 136-143页

作者： ZABIK, ME HOOJJAT, P WEAVER, CM 1. Department of Food Science and Human Nutrition Michigan State University 48824 East Lansing Mich.

Recent data show that polychlorinated biphenyl (PCB) concentrations in a particular type of lake trout (Salvelinus namaycush) caught in Lake Superior are excessively high. This type of trout is often referred to as fat trout or siscowets by local fishermen and have been found to have over 30 ppm of PCBs in the edible fillet. The objective of this study was to determine the effect of cooking fat trout fillets by broiling, baking and microwave on the levels of PCBs and other organochlorine pesticides. Sections of whole trout were also roasted with and without skin to determine the effect of removal with and without skin to determine the effect of removal of skin and the adhering fat on the levels of these contaminants in the edible flesh. Roasting trout pieces without skin resulted in an average of 50% loss of PCBs, 57% of dieldrin, and 57% of DDT compounds while roasting trout pieces with skin resulted in an average of 40% loss of PCBs, 45% of dieldrin and 47% of DDT compounds from the edible flesh. Although these differences are not statistically significant, it can certainly be recommended to remove the skin and associated fat before cooking this type of fish.

关键词：烹饪滴滴涕/分析狄氏剂/分析肉/分析农药残留量/分析多氯联苯化合物/分析鲑科鳟动物

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Determination of organochlorine pesticide residues in medicinal plants sold in Coimbra, Portugal

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JOURNAL OF AOAC INTERNATIONAL 1999年第5期82卷 1206-1213页

作者： Lino, CM Guarda, LMC Silveira, MIN Univ Coimbra Fac Pharm Lab Bromatol & Hydrol P-3000 Coimbra Portugal

Levels of 14 organochlorine pesticide residues-1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane (DDT) group (p,p'-DDT, o,p'-DDT, p,p'-DDD, and p,p'-DDE), HCH isomers (alpha-, beta-, and gamma-HCH), hexachlorobenzene (HCB), aldrin, dieldrin, endrin, heptachlor, alpha-endosulfan, and endosulfan sulfate-were evaluated in 127 samples of medicinal plants collected in pharmacies (78 samples) and herb stores (49 samples) in 1996. Samples were divided between 15 national brands and 7 foreign brands, Most samples sold in pharmacies contained residues of gamma-HCH (51.3%). All residues were detected in analyzed samples, with exception of endrin in herb store samples. Detection frequency varied between 51.3% for gamma-HCH and 1.3% for endrin in pharmacy samples, and between 34.7% for HCB and 4.1% for endosulfan sulfate in herb store samples. Maximum residue levels were exceeded in 38 (48.7%) pharmacy samples and in 26 (53.1%) medicinal herb store samples.

关键词：烃类氯化杀虫药/分析农药残留量/分析植物药用/化学葡萄牙

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