Tiêu chuẩn Việt Nam TCVN 5142:2008 (CODEX STAN 229-1993, Rev.1-2003) về phân tích dư lượng thuốc bảo vệ thực vật - các phương pháp khuyến cáo

TIÊU CHUẨN VIỆT NAM

TCVN 5142:2008

PHÂN TÍCH DƯ LƯỢNG THUỐC BẢO VỆ THỰC VẬT – CÁC PHƯƠNG PHÁP KHUYẾN CÁO

Analysis of pesticide residues – recommended methods

Lời nói đầu

TCVN 5142:2008 thay thế TCVN 5142:1990 ;

TCVN 5142:2008 hoàn toàn tương đương với CODEX STAN 229-1993, Rev.1-2003;

TCVN 5142:2008 do Ban kỹ thuật tiêu chuẩn TCVN/TC/F13 Phương pháp phân tích và lấy mẫu biên soạn, Tổng cục Tiêu chuẩn Đo lường Chất lượng đề nghị, Bộ Khoa học và Công nghệ công bố.

PHÂN TÍCH DƯ LƯỢNG THUỐC BẢO VỆ THỰC VẬT – CÁC PHƯƠNG PHÁP KHUYẾN CÁO

Analysis of pesticide residues – recommended methods

1. Giới thiệu

1.1. Phạm vi áp dụng

Các phương pháp phân tích liệt kê dưới đây được tổng kết từ kinh nghiệm thực hành của Ủy Ban Codex về Dư lượng Thuốc bảo vệ thực vật, được xem xét để xác định dư lượng thuốc bảo vệ thực vật theo quy định. Danh mục đưa ra trong điều 2 chưa đề cập hết mọi khía cạnh và có thể áp dụng các phương pháp không có trong danh mục này miễn là chúng có thể cho kết quả chính xác khi sử dụng các phương pháp đó.

1.2. Tiêu chí để lựa chọn phương pháp phân tích

Bất cứ khi nào có thể, việc lựa chọn phương pháp phân tích dư lượng thuốc bảo vệ thực vật được dựa trên các tiêu chí sau đây:

i. Sẵn có các tài liệu tạp chí, sổ tay hoặc trên mạng điện tử của các tổ chức tiêu chuẩn quốc tế hoặc quốc gia;

ii. Đã có sự nghiên cứu phối hợp của một số phòng thí nghiệm hoặc đã được kiểm tra xác nhận. Việc kiểm tra xác nhận phương pháp đối với phòng thí nghiệm riêng rẽ tối thiểu đã tuân thủ hướng dẫn thực hành tốt về phân tích dư lượng thuốc bảo vệ thực vật.

iii. Có khả năng xác định nhiều hơn một loại thuốc bảo vệ thực vật, nghĩa là phương pháp đa dư lượng;

iv. Thích hợp cho nhiều loại sản phẩm có nồng độ dưới mức quy định MRLs;

v. Có thể áp dụng đối với các phòng thí nghiệm được trang bị các thiết bị, dụng cụ phân tích có sẵn thông thường.

Ưu tiên sử dụng sắc ký khí hoặc sắc ký lỏng hiệu năng cao như là bước tách chiết của các phương pháp. Tuy nhiên, trong các điều kiện xác định, phương pháp sàng lọc quy định trong hướng dẫn thực hành tốt về phân tích dư lượng thuốc bảo vệ thực vật có thể áp dụng. Phương pháp sàng lọc được chỉ ra trong danh mục.

1.3. Áp dụng phương pháp

Trước khi áp dụng phương pháp cần phê chuẩn phương pháp và chứng minh năng lực của người phân tích. Trong quá trình sử dụng, định kỳ cần phải đánh giá xác nhận các đặc tính của phương pháp. Việc phê chuẩn và xác nhận đặc tính của phương pháp được mô tả trong Hướng dẫn thực hành tốt về phân tích dư lượng.

1.4. Tài liệu tham khảo

Các khuyến cáo liên quan khác của Codex về giới hạn tối đa dư lượng thuốc bảo vệ thực vật thuộc phạm vi bắt buộc như sau:

1. Các phương pháp lấy mẫu khuyến cáo để xác định dư lượng thuốc bảo vệ thực vật (tham khảo Codex Alimentarius tập 2, chương 3).

2. Bộ phận hàng hóa áp dụng giới hạn dư lượng tối đa và được dùng để phân tích [tham khảo TCVN 5140:2008 (Volume 2A, Part 1 – 2000)].

3. Các giải thích về giới hạn tối đa về dư lượng thuốc bảo vệ thực vật của Codex (tham khảo Codex Alimentarius tập 2, chương 1).

4. Hướng dẫn thực hành tốt khi phân tích dư lượng thuốc bảo vệ thực vật của Codex (tham khảo Codex Alimentarius phần bổ sung 1, tập 2, chương 4).

Ở 3 đoạn của tài liệu tham khảo có thể tìm thấy:

● Các bài báo chung về phương pháp luận đối với dư lượng thuốc bảo vệ thực vật (đoạn 3.1);

● Sổ tay (đoạn 3.2);

● Các bài báo cụ thể (đoạn 3.3).

Sau mỗi tài liệu tham khảo trong đoạn 3.3, các hợp chất liên quan đến áp dụng các phương pháp phân tích được chỉ ra bằng số CCPR của chúng.

2. Danh mục các phương pháp phân tích

Các số hiệu đối với sổ tay và sách được liệt kê trong 3.2, tên đối với tác giả (thứ nhất) của các bài báo được liệt kê trong đoạn 3.3.

3. Tài liệu tham khảo

3.1. Các bài báo chung

Các bài báo hoặc sách liên quan đến các vấn đề về phân tích dư lượng thuốc bảo vệ thực vật (xem thêm sổ tay đã được viện dẫn trong đoạn 3.2).

Ambrus, A. & Thier, H.-P., Application of multi-residue procedures in pesticides residues analysis, Pure Appl. Chem., 58, 1035-1062 (1986).

Beck, H., Untersuchungsmethoden zur Bestimmung der Ruckstande von Chlorkohlenwasserstoff- Pestiziden in oder auf Lebensmitteln, Bundesgesundheitsblatt, 17, 269-274 (1974).

Becker, G. et al., Dunnschichtchromatographie in der Ruckstandsanalytik von Pflanzenschutzmitteln und deren Metaboliten, Verlag Chemie VCH, Weinheim, FRG (1987).

Burke. J.A., The interlaboratory study in pesticide residue analyses, in: Advances in Pesticide

Science, H. Geissbuehlor (edit.), Pergamon Press, Oxford, UK, 633-642 (1979).

Carl, M., Internal laboratory quality control in the routine determination of chlorinated pesticides, in: Advances in Pesticide Science, H. Geissbuehler (edit.), Pergamon Press, Oxford, UK, 660-663 (1979).

Cochrane, W.P., Chemical derivatization in pesticide analysis, Plenum Press, New York, N.Y., USA, (1981).

Egli, H., Storage stability of pesticide residues, J. Agr. Fd. Chem., 30, 861-866 (1982)

Frehse. H. & Timme. G., Quantitative residue analytical reliability: beatitude through the application of latitude, Res. Revs., 73, 27-47 (1980).

Gunther, F.A., Interpreting pesticide residue data at the analytical level, Res. Revs., 76, 155-171 (1980).

Horwitz, W., The role of the analyst in analytical chemistry, FDA Bylines, 4. 169-178 (1979).

Horwitz, W., The inevitability of variability in pesticide residue analysis, in: Advances in Pesticide Science. H. Geissbuehler (edit.), Pergamon Press, Oxford, UK, 649-655 (1979).

Horwitz, W. et al., Quality assurance in the analysis of foods for trace constituents, JAOAC, 63, 1344-1354(1980).

Horwitz, W., Evaluation of analytical methods used for regulation of foods and drugs, Anal. Chem., 54, 67A-76A (1982).

ISO Document ISO 5725, 2nd edit. (1986), Precision of test methods: determination of repeatability and reproducibility.

IUPAC Reports on Pesticides (13), Development and evaluation of simplified approaches to residues analysis, Pure Appl. Chem., 53. 1039-1049 (1981).

Moye, H.A. (edit.), Analysis of pesticide residues, Vol. 58 of: Chemical Analysis, John Wiley and Sons, New York, N.Y., USA (1981).

Pesticide Residue Analysis, Health Aspects of Chemical Safety, Interim Document 14, WHO, Regional Office for Europe, Copenhagen, Denmark (1984).

Safe, S. & Hutzinger, O., Mass spectrometry of pesticides and pollutants, CFC Press Inc., Boca Raton, Florida, USA (1979).

Smart, N., Samples used for interlaboratory studies of methods for pesticide residues analysis in foodstuffs, Res. Revs., 96, 1-12 (1985).

Steiner, E.H., Planning and analysis of results of collaborative tests, in: Statistical Manual of the AOAC, Washington, D.C., USA (1974).

The Agrochemical Handbook, The Royal Society of Chemistry, The University, Nottingham, UK, (1983).

Thier, H.-P. & Frehse, H., Rỹckstandsanalytik von Pflanzenschutzmitteln, Georg Thieme Verlag, Stuttgart - New York (1986).

Youden. W.J., Statistical techniques for collaborative tests, in: Statistical Manual of the AOAC, Washington, D.C., USA (1974).

Zweig, G. (edit.), Analytical methods for pesticides, plant growth regulators and food additives Academic Press, New York - San Francisco - London, Vol.  XIV and XV (1986).

3.2. Sổ tay

(1) Official Methods of AOAC INTERNATIONAL, 16th edition (1995)

(2) Pesticide Analytical Manual, Food and Drug Administration, Washington, D.C., USA

(3) Manual on Analytical Methods for Pesticide Residues in Foods, Health Protection Branch, Health and Welfare Canada, Ottawa, Ont., Canada (1985) (available in English and French)

(4) Methodensammlung zur Rỹckstandsanalytik von Pflanzenschutzmitteln, 1.- 11. Lieferung, VCH Verlagsgesellschaft, Weinheim, FRG (1991) (the numbers in parentheses refer to the numbers of the methods in this manual; methods preceeded by "S" are multi-residue methods; the manual is also available in English, see ref. 7).

(5) Laboratory Manual for Pesticide Residues Analysis in Agricultural Products, compiled by R.B. Maybury, Pesticide Laboratory, Food Production and Inspection Branch, Agriculture Canada, Ottawa, Ont., Canada (1984) (available in English and French).

(6 ) Zweig, G. (edit.), Analytical Methods for Pesticides, Plant Growth Regulators , Academic Press, New York - San Francisco - London

(7) Manual of Pesticide Residue Analysis, Deutsche Forschungsgemeinschaft, VCH Verlagsgesellschaft, Weinheim, FRG (1987) (English translation of ref. 4)

(8) Chemistry Laboratory Guidebook, United States Department of Agriculture, Food Safety and Inspection Service, Science Program, Washington, D.C., USA

(9) Analytical Methods for Residues of Pesticides in Foodstuffs, P.A. Greve (edit.), 5th edition. Government Publishing Office, The Hague, Netherlands (1988)

(a) Part I: Multi-residue Methods (the numbers in parentheses refer to numbers of themulti-residue methods in this volume)

(b) Part II: Special Methods (methods given under compound name)

(10) Materials and Methods Used for Pesticide Residues Monitoring in Sweden, Var Foda, 38, Suppl.2, 79-136 (1986)

(11) Comprehensive Analytical Profiles of Important Pesticides (Modern methods for pesticides analysis) e.d. J. Sherma & T Cairns 1992.

3.3. Bài báo cụ thể

The numbers in italics after the references refer to the compounds, indicated by their CCPR- number, to which the methods involved apply.

Abbott (1), D.C. et al., Pest. Sci., 1. 10-13 (1970)

Pesticide residues in the total diet in England and Wales, 1966-1967; Part III: Organophosphorus pesticide residues in the total diet

2, 4, 5, 11,14,22,25,27,28,34,36, 37,39,42,49,53,55, 58, 59, 60, 66, 68,73, 74, 76, 92,112, 124

Abbott (2). D.C. et al., J. Chromatog., 16, 481-487 (1964)

Some observations on the thin-layer chromatography of organochlorine pesticides

1,21,32,33,43,48

Adachi, K. et al., JAOAC, 67, 798-800 (1984)

Simple analytical method for organophosphorus pesticide determination in unpolished rice, using removal of fats by zinc acetate

22,27,37,49,58,128

Adler, I.L. & Wargo Jr, J.P., JAOAC, 58, 551-553 (1975)

Determination of residues from the herbicide 2,4-dichloro-1-(4-nitrophenoxy)-benzene in rice and wheat by electron-capture gas-liquid chromatography

140

Aharonson, N. & Muszkat. L., Z. Lebensm. Unters. Forsch., 180, 96-100 (1985)

Direct gas chromatographic determination of the two isomeric insecticides, aldicarb and butocarboxime and their toxic metabolites: application to residue analysis in crops and leaves

117,139

Allen (1), J.G. & Hall. K.J., J. Agr. Fd. Chem., 28, 255-258 (1980)

Methods for the determination of diphenylamine residues in apples

30

Allen (2), J.G., Pest. Sci., 11,347-350(1980)

Daminozide residues in sWeet cherries, and their determination by colorimetric and gas-liquid chromatographic methods

104

Allmendinger H. Pflanzensch. Nachr. Bayer, 44, 5-66 (1991)

A method for determining residues of the fungicides folicur and Bayfidan in plant material and soil by gas chromatography.

168,189

Ambrus, A. et al., JAOAC, 64, 733-768 (1981)

General method for determination of pesticide residues in samples of plant origin, soil, and water

1,2,4,6,7,8,14,17,21,22,25,27,32,33, 37,39,41,42,43,48,49, 51,53,54,58,59,60,61, 66, 73, 74,75, 76, 77, 80, 81, 82, 83, 86,87, 94, 96,101, 103, 112,113, 117,118, 119, 120, 123, 128, 133, 135, 137, 140,141, 143,159

Andersson, A and Ohlin, B. Vồr Fửda 38, 79-109 (1986)

A capillary gaschromatographic multiresidue method for the determination pesticide residues in fruit and vegetables.

162, 164,168, 171

Austin, D.J. & Hall, K.J. Pest. Sci., 12, 495-502 (1981)

A method of analysis for the determination of binapacryl, bupirimateand diflubenzuron on apple foliage and fruit, and its application to persistence studies

3,130

Baker, P.B. (1) & Flaherty. B., Analyst, 97, 713-718 (1972)

Fungicide residues; Part II: The simultaneous determination of residues of folpet, captan and captafol in selected fruits by gas chromatography

6, 7, 41

Baker, P.B. (2) & Hoodless, R.A., Analyst, 98, 172-175 (1973)

Fungicide residues; Part III: The determination of binapacryl in selected fruits by gas chromatography

3

Baker, P.G. (1) et al., Analyst. 105, 282-285 (1980)

Fungicide residues; Part VII: Determination of residues of fentin in vegetables and cocoa products by spectrofluorimetry

40

Baker, P.G. (2) & Bottomley, P., Analyst, 107, 206-212 (1982)

Determination of residues of synthetic pyrethroids in fruit and vegetables by gas-liquid and high-performance liquid chromatography

93, 118, 119, 120, 127, 135

Baker, P.G. & Clarke, P.G., Analyst 109, 81-83 (1984)

Determination of residues of dithianon in apples by HPLC

Bardalaye, C, Wheeler, W.B. & Meister C.W. JAOAC 70, 455-457 (1987)

Gas chromatographic determination of cyromazine and its degradation product melamine in chinese cabbage.

169

Becker, G., Schug, P., Deutsche Lebensm. Rundschau 86, 239-242 (1990)

Eine miniaturmethode zur schnellen Bestimmung von Pestizidrỹckstonden in pflanzlichen Lebensmitteln.

191

Bichi, C. et al. Pestic. Sci. 30. 13-19 (1990)

Simultaneous determination of clofentezine, fenoxycarb and hexthiazox by HPLC on apples, pears and their pulps

156

Bottomley, P. & Baker, P.G., Analyst, 109, 85-90 (1984)

Multi-residue determination of organochlorine, organophosphorus and synthetic pyrethroid pesticides in grain by gas-liquid and high-performance liquid chromatography

1, 4, 21, 22, 25, 37, 44, 49, 61, 66, 86, 90, 93, 118, 119, 120. 123, 127, 135

Bourke, J.B. et al., J. Agr. Fd. Chem., 25, 36-39 (1977)

Residues and disappearance of triforine from various crops

116

Brauckhoff, S. & Thier, H.-P., Z. Lebensm. Unters, Forsch.,_; 184, 91-95 (1987)

Analysenmethode fỹr Rỹckstọnde von Methylcarbamat-lnsecticiden in pflanzlichen Lebensmitteln

8, 75, 94, 96, 101, 107, 117, 132, 134, 137, 139

Brennecke (1), R., Pflanzensch. Nachr. Baycr, (Engl. edit.)38, 33-54 (1985)

Method for gas-chromatographic determination of residues of Baycor fungicide in plant material, soil and Water (Engl. edit.: 38, 33-54 (1985))

144

Brennecke (2), R., Pflanzensch. Nachr. Bayer, 37, 68-93 (1984)

Method for gas-chromatographic determination of residues of Bayleton and Bayfidan fungicides in plant material, soil and Water (German edit.: 37, 66-91 (1984))

133, 168

Brennccke (3), R., Pflanzensch. Nachr. Bayer, 41,113-131 (1988)

Method for the determination of residues of the fungicide Baycor in plant material and beverages by high pressure liquid chromatography with fluorescence detection (German edit.: 41, 113-135 (1988))

144

Brennecke (4), R., Pflanzensch. Nachr. Bayer, 41, 137-174 (1988).

A method for the determination of residues of the fungicides Euparen and Euparen M in plant material and beverages by gaschromatography (German edit. 41. 136-172 (1988)).

82,162

Brennecke (5), R., Pflanzensch. Nachr. Bayer. 38, 11-32 (1985)

Method for gas-chromatographic determination of Dyrene residues in plant material, soil and water (German edit.: 38, 11-32 (1985)).

163

Brennecke (6), R., Pflanzensch. Nachr. Bayer, 42, 223-284 (1989) German edit.

A method for determining residues of the fungicides Euparen, Euparen M and Folicur in plant material and beverages by gaschromatography.

189

Buettler, B. & Hoermann, W.D., J. Agr. Fd. Chem., 29, 257-260 (1981)

High-pressure liquid chromatographic determination of captan, captafol, and tolpet residues in plant material

6, 7, 41

Cabras, P., Meloni, M., & Spaneddal, J. Chromatogr. 505, 413-416 (1990)

High-performance liquid chromatographic separation of cyromazine and its metabolite melamine.

169

Calderbank (1), A. & Yuen, S.H., Analyst, 90, 99-106 (1965)

An ion-exchange method for determining paraquat residues in food crops

57

Calderbank (2), A. & Yuen, S.H., Analyst, 91, 625-629 (1966)

An improved method for determining residues of diquat

31

Cessna, A.J. J.Agr.Fd.Chem. 33, 108-110 (1985)

Gas chromatograohic analysis of the herbicide bentazone in leeks

172

Chaput, D. JAOAC, 71, 542-546. (1988)

Simplified multiresidue method for liquid chromatographic determination of N-methylcarbamate insecticides in fruits and vegetables.

8, 75, 94, 96, 117, 132

Cochrane, W.P. et al., JAOAC, 59, 617-621 (1976)

Gas-liquid chromatographic analysis of ethephon and fenoprop residues in apples and their decline before and after harvest

106

Conditt, M et al, JAOAC, 71, 735-739 (1988).

Gas chromatography/mass spectrometric determination of daminozide in high protein food products.

104

Cowell, J.E., Kunstman, J.L., Nord, P.J., Steinmetz, J.R. and Wilson, G.R. J. Agric. Fd. Chem. 34, 955- 960(1986)

Validation of an analytical method for analysis of glyphosate and Metabolite: An interlaboratory study

158

Daft, J.L., JAOAC. 66, 228 (1983)

Gas chromatographic determination of fumigant residues in stored grains, using isooctane partitioning and dual column packings

10, 23, 24

Day, E.W. et al., JAOAC, 51. 39-44 (1968)

Determination of sec-butylamine residues in fruit

89

Desmarchelier, J. et al., Pest. Sci., 8, 473-483 (1977)

A collaborative study of residues on Wheat of chlorpyrifos-methyl, fenitrothion, malathion, methacrifos and pirimiphos-metyl

37,49,86,90,125

Dieckmann H. et al, Fresenius J. Anal. Chem. 345, 784-786 (1993)

Simultaneous determination of fenpropimorph and the corresponding metabolite fenpropimorphic acid in soil.

188

Ebing, W. et al., Lebensm. gerichtl. Chem., 39. 126-130 (1985)

Zur Ruckstandsanalytik von Phenoxyalkancarbonsoure-Herbiziden in Getreidekornern

20, 121

Farrow, J.E. et al., Analyst, 102. 752-758 (1977)

Fungicide residues; Part VI: Determination of residues of post-harvest fungicides on citrus fruit by high-performance liquid chromatography

29, 56, 65, 72

Francoeur, Y. & Mallet, V., JAOAC, 59, 172-173 (1976)

Determination of quinomethionate (6-methylquinoline-2,3-diyldithiocarbamate) residues in crops by in situ fluorimetry

80

Galoux, M. et al.. JAOAC, 65, 24-27 (1982)

Colorimetric determination of 3-amino-1,2,4-triazole in grain or meal

79

Gentile, I.A. & Passera. E., J. Chromatog., 236, 254-257 (1982)

Separation and detection of propamocarb by thin-layer chromatography

148

Gilvydis, D.M. & Walters, S.M., JAOAC, 67, 909-912 (1984)

Determination of captan, folpet, and captafol in fruits and vegetables, using two multiresidue methods

6, 7, 41

Heikes, D.L., JAOAC, 68, 431-436 (1985)

Purge and trap method for determination of ethylene dibromide in table-ready foods

23

Hill, A.R.C. et al., Analyst, 109, 483-487 (1984)

Organophosphorus sulphides, sulphoxides and sulphones; Part I: Determination of residues in fruit and vegetables by gas-liquid chromatography

38,39,73,74,76,85, 112

Hirvi, T. et al., J. Agr. Fd. Chem., 27, 194-195 (1979)

A glass capillary gas-liquid chromatography method for determining ethylenethiourea Without derivatization

108

Hogendoorn, E.A. and Goewie, C.E. J. Chromatogr. 475, 432-441 (1989)

Residue analysis of the herbicides cyanizine and bentazone in sugar maize and surface water using high-performance liquid chromatography and an on-line clean-up column-sitching procedure

172

Hunter, K. & Lindsay, D., Pest. Sci., 12, 319-324 (1981)

High-pressure liquid chromatographic determination of sec-butylamine residues in potatoes

89

Ishii, Y. (1) et al., J. Pest. Sci., 15, 205-209 (1990)

Clean up procedure for determination of pesticide residues in crops using charcoal - Florisil mini column Ishii, Y. (2) et al., J. Pest. Sci. 15, 231-236 (1990)

Residue analysis of organochlorine pesticides by GC equipped with a Hall electrolytic conductivity detector (Halogen mode)

191

Kadenczki, L., et al, JAOAC 75, 53-61 (1992)

Column extraction of residues of several pesticides from fruits and vegetables: A simple multi residue analysis method

Khan, S.U., Bull. Envir. Cont. Tox., 14, 745-749 (1975)

Determination of paraquat residues in food crops by gas chromatography

57

King, R.R., J. Agr. Fd. Chem., 26, 1460-1463 (1978)

Gas chromatographic determination of diquat residues in potato tubers

31

Kitada, Y. et al., JAOAC, 65, 1302-1304 (1982)

Simultaneous liquid chromatographic determination of thiabendazole, o-phenylphenol, and diphenyl residues in citrus fruits, Without prior cleanup

29, 56, 65

Kobayashi, H. et al., J. Pest. Sci., 2. 427-430 (1977)

Gas chromatographic determination of guanidino fungicide, guazatine, in rice grain

114

Krause (1), R.T. & August, E.M., JAOAC, 66, 1018-1022 (1983)

Applicability of a multiresidue method and high performance liquid chrornatography for the determination of chinomethionate in apples and oranges

80

Krause (2), R.T. & August, E.M., JAOAC, 66. 234-240 (1983)

Applicability of a carbamate insecticide multiresidue method for determining additional types of pesticides in fruits and vegetables

62

Lafuente (1) M.T. et al, JAOAC 69, 859-862 (1986) GC determination of fenpropimorph residues in citrus fruit

8

Lafuente (2) M.T. et al, Fres. J. Anal. Chem. 328, 105-107 (1987) GLC multiresidue analysis of postharvest fungicides in citrus fruit

188

Lane (1). J.R., JAOAC, 46, 261-268 (1963) Collaborative study of maleic hydrazide residue analysis

102

Lane (2), J.R., JAOAC, 48, 744-748 (1965)

Collaborative study of maleic hydrazide residue analysis

102

Lawrence(1), J.F., J. Agr. Fd. Chem., 25. 211-212 (1977)

Direct analysis of some carbamate pesticides in foods by high-pressure liquid chromatography

8, 75,96

Lawrence (2), J.F. & Panopio, L.G. JAOAC 63, 1300-1303 (1980)

Comparison of gas and liquid chromatography for determination of anilazine in potatoes and tomatoes.

163

Lembo, S. et al., J. Chromatog., 267, 427-430 (1983)

Gas-liquid chromatographic method for determining propylenethiourea in rat tissues and fluids

150

Leppert (1), B.C. et al., J. Agr. Fd. Chem., 31, 220-223 (1983)

Determination of carbosulfan and carbofuran residues in plants, soil, and Water by gas chromatography

145

Leppert (2), B.C. et al., J. Agr. Fd. Chem., 32, 1441 (1984) Comment on recovery of carbosulfan residues from acidic crops

145

Li Yu-Chang et al., Fres. Z. Anal. Chem., 316, 290-292 (1983)

Methode zur Bestimmung von Rỹckstọnden an Butocarboxim in Pflanzen und Boden mit Hilfe der HPLC

139

Lokke (1), H., J. Chromatog., 200, 234-237 (1980) Determination of amitrole by ion-pair high-performance liquid chromatography

79

Lokke (2), H., J. Chromatog., 179, 259-270 (1979) Investigation on loss of chlorothalonil, dichlofluanid, tolylfluanid and vinclozolin by column chromatography clean-up on silver-loaded alumina in a gas chromalographic multiresidue procedure

81, 82

Lokke (3), H. & Odgaard, P., Pest. Sci., 12, 375-384 (1981)

Residues in blackcurrants, fodder peas, spinach and potatoes treated with sublethal doses of 2,4,5-T to simulate wind drift damage

121

Lord, E. et al., J. Assoc. Publ. Anal., 16, 25-32 (1978)

The determination of biphenyl and 2-hydroxybiphenyl in citrus fruit

29, 56

Lott, P.F. et al., J. Chromat. Sci., 16, 390-395 (1978)

The determination of paraquat

57

Love, J.L. & Patterson, J.E., JAOAC, 61, 627-628 (1978)

Atomic absorption spectrometric determination of cyhexatin

67

Lubkowitz, J.A. et al., J. Agr. Fd. Chem., 21, 143-144 (1973)

Residue studies of O.S-dimetylphosphoroamidothioate on tomatoes

100

Luke. B.G. & Cossens, S.A., Bull. Envir. Cont. Tox., 24, 746-751 (1980)

Determination of diphenylamine residues in apples

30

Maasfeld, Pflanzenschutz Nachr. Bayer 40, 29-48 (1987) German Ed.

Method for GC determination of residues of the fungicide Folicur in plant material

189

Maclaine Pont, M.A. etal., Meded. Fac. Landbouww. Rijksuniv. Gent, 45, 835-840 (1980)

The residue analysis of prochloraz in combination with dicloran

142

Mendes, M.C.S. J. Agric. Fd. Chem. 38 174-178 (1990)

Evaluation and confirmation of acetylation gas liquid chromatographic method for the determination of triadimenol in foods.

168

Mestres (1), R. et al., Trav. Soc. Pharm. Montpellier, 35, 87-100 (1975)

Méthode rapide de contrôle et de dosage des résidus d’ortho-phényl phénol et de biphényle dans les agrumes

29, 56, 72, 77

Mestres (2), R. et al., Ann. Fals. Exp. Chim., 73, 407-420 (1980)

Méthode de recherche et de dosage des résidus de pesticides dans les produits céréaliers; 2o: Fumigants

9, 10, 23, 24, 52

Mestres (3), R. et al., Proc. Int. Soc. Citricult., 3, 1103-1106 (1977)

Thiophanate-metylpostharvest residues in oranges

65, 72, 77

Moellhoff (1), E., Pflanzensch. Nachr. Bayer (Engl. edit.). 28, 370-381 (1975)

Method for gas-chromatographic determination of Curaterr residues in plants and soil samples With consideration to metabolites

96

Moellhoff (2), E., Pflanzensch. Nachr. Bayer (Engl. edit.), 30, 249-263 (1977)

Method for gas-chromatographic determination of Peropal acaricide and its metabolites in plants, soil, Water and laboratory animal chow

67, 129

Muszkat, L. & Aharonson, N., J. Chromat. Sci.. 21, 411-414 (1983)

GC/CI/MS analysis of aldicarb, butocarboxime, and their metabolites

117, 139

Nakamura et al., J. AOAC 76, 1348-1361 (1993)

Determination of pyrethroid residues in vegetables, fruits, grains, beans and green tea.

185

Newsome (1). W.H., J. Agr. Fd. Chem., 24, 997-999 (1976)

A gas-liquid chromatographic method for the determination of dodine residues in foods

84

NeWsome (2). W.H., J. Agr. Fd. Chem., 22. 887-889 (1974)

A method for determining ethylenebis(dithiocarbamate) residues on food crops as bis(trifluoro-acetamido) ethane

105

Newsome (3), W.H., J. Agr. Fd. Chem., 28, 270-272 (1980)

A method for the determination of maleic hydrazide and its b-D-glucoside in foods by high-pressure anion-exchange liquid chromatography

102

Newsome (4). W.H., J. Agr. Fd. Chem., 30, 778-779 (1982)

Determination of triforine in fruit crops as N,N’-bis(pentafluorobenzoyl)piperazine

116

NeWsome (5), W.H., J. Agr. Fd. Chem., 28, 319-321 (1980)

Determination of daminozide residues on foods and its degradation to 1,1-dimethylhydrazine by cooking

104

Nishizawa, H., et al, JAOAC accepted for publication

Simple clean-up procedure for residue analysis of buprofezin and its metabolites in crops by GC Nitz, S. et al., J. Agr. Fd. Chem., 30, 593-596 (1982)

A capillary gas-liquid chromatographic method for deterrnination of ethylenethiourea and propylene thiourea in hops, beer, and grapes

108, 150

Official Gazette, no. 4 of the Notification issued on March 20, 1979, by the Japan Environment Agency Residue analysis of cartap hydrochloride

97

Ott, D.E. & Gunther, F.A., JAOAC, 909-912 (1982)

Field screening method for above-tolerance residues of dithiocarbamate fungicides

105

Otto. S. et al., J. Envir. Sci. Health, Part B, 12, 179-191 (1977)

A new gas chromatographic determination of ethylene thiourea residues without derivatization

108

Panel (1) of the Committee for Analytical Methods for Residues of Pesticidos and Veterinary Products in Foodstuffs of the Ministry of Agriculture, Fisheries and Food, Analyst, 98, 19-24 (1973)

The determination of malathion and dichlorvos residues in grain

25, 49

Panel (2) of the Committee for Analytical Methods for Residues of Pesticides and Veterinary Products in Foodstuffs of the Ministry of Agriculture, Fisheries and Food, Analyst, 101, 386-390 (1976)

Determination of residues of inorganic bromide in grain

4

Panel (3) of the Committee for Analytical Methods for Residues of Pesticides and Veterinary Products in Foodstuffs of the Ministry of Agriculture. Fisheries and Food, Analyst, 102, 858-868 (1977)

Determination of residues of organophosphorus pesticides in fruits and vegetables

2, 27,49,55,58

Panel (4) of the Committee for Analytical Methods for Residues of Pesticides and Veterinary Products in Foodstuffs of the Ministry of Agriculture, Fisheries and Food, Analyst, 104, 425-433 (1979)

Determination of organochlorine pesticides in animal fats and eggs

1,21,33,44,48

Panel (5) of the Committee for Analytical Methods for Residues of Pesticides and Veterinary Products in Foodstuffs of the Ministry of Agriculture, Fisheries and Food, Analyst, 99, 570-576 (1974)

The determination of residues of volatile fumigants in grain

10, 23

Panel (6) of the Committee for Analytical Methods for Residues of Pesticides and Veterinary Products in Foodstuffs of the Ministry of Agriculture, Fisheries and Food, Analyst, 106, 782-787 (1981)

Determination of residues of dithiocarbamate pesticides in foodstuffs by a headspace method

105

Panel (7) of the Committee for Analytical Methods for Residues of Pesticides and Veterinary Products in Foodstuffs of the Ministry of Agriculture, Fisheries and Food, Analyst, 105, 515-517 (1980)

Determination of a range of organophosphorus pesticide residues in grain

4,22,27,37,49,74,86,112

Panel (8) of the Committee for Analytical Methods for Residues of Pesticides and Veterinary Products in Foodstuffs of the Ministry of Agriculture, Fisheries and Food, Analyst, 110, 765-768 (1985)

Determination of a range of organophosphorus pesticide residues in grain

4, 27, 37, 49, 86, 90,123, 125

Panel (9) of the Committee for Analytical Methods for Residues of Pesticides and Veterinary Products in Foodstuffs of the Ministry of Agriculture, Fisheries and Food, Analyst, 112, 1559-1563 (1987)

Determination of ethylenethiourea in canned fruits and vegetables

108

Phillips, A.J.L., Phytophylactica 24 289-292 (1992). Bioassay of tolclofos-metylin bean seed.

191

Player, R.B. & Wood. R., J. Assoc. Publ. Anal., 18, 109-117 (1980)

Methods of analysis - collaborative studies; Part III: Determination of biphenyl and 2-hydroxy-biphenyl in citrus fruit

29,56

Van der Poll, J.M., Vink, M. and Quirijns, J.K. Chromatographia, 30, 155-158, 1990.

Determination of amitrole in plant tissues and sandy soils by capillary gaschromatography With alkali flame ionization detection.

79

Pomerantz, I.H. & Ross. R., JAOAC, 51. 1058-1062 (1968)

Captan and structurally related compounds: thin layer and gas-liquid chromatography

6, 7, 41

Prabhu, S.V., Varsolona, R.J., Welmer. T.A. , Egan, R.S. and TWay, P.C. J. Agr. Fd. Chem. 40,622-625 (1992)

Rapid and sensitive high performance liquid chromatographic method for the quantificxation of abamectine and its delta 8,9 isomer.

177

Pyysalo, H. et al., J. Chromatog., 168, 512-516 (1979)

Extraction and determination of o-phenylphenol and biphenyl in citrus fruits and apples

29, 56

Ragab, M.T.H. Anderson, M.G. & Johnston, H.W. Bull Envir. Contam. Toxicol. 44, 100-105 (1990)

Residue analysis of triadimefon, triadimenol and the BAY KWG1342 diol and BAY KWG1323 hydroxylated matabolites in winterweed.

133,168

Rains, D.M. & Holder, J.W., JAOAC, 64, 1252-1254 (1981)

Ethylene dibromide residues in biscuits and commercial flour

23

Rajzman, A., Analyst, 99, 120-127 (1974)

Determination of thiabendazole in citrus fruits by ultraviolet spectrophotometry

65

Reed, A.N., J. Chromatogr. 438, 393-400 (1988)

Quantification of triazole and pyrimidine plant growth retardants

161

Rosenberg, C. & Siltanen, H., Bull. Envir. Cont. Tox., 22, 475-478 (1979)

Residues of mancozeb and ethylenethiourea in grain samples

108

Roughan, J.A. et al., Analyst, 108, 742-747 (1983)

Modifíed gas-liquid chromatographic method for determining bromide/total bromine in foodstuffs and soils

47

Sachse, J., Z. Lebensm. Unters. Forsch., 163, 274-277 (1977)

Uber die Bestimmung von Chlorcholinchlorid (CCC) in Getreide

15

Sano, M. et al., JAOAC, 62, 764-768 (1979)

Flameless atomic absorption spectrophotometric determination of Vendex, an organic tin miticide, in apples, oranges, and tea leaves

109

Saxton W.L et al. J. Agric. Food Chem., 37, 570-573 (1989)

Results of a survey for the presence of daminozide and unsymmetrical dimethylhydrazine in food.

104

Scudamore (1), K.A., Analyst, 105, 1171-1175(1980)

Determination of 2-aminobutane in potatoes using high-performance liquid chromatography

89

Scudamore (2), K.A. & Goodship, G., Pest. Sci., 17, 385-395 (1986)

Determination of phosphine residues in fumigated cereals and other foodstuffs

46

Snowdon, P.G., et al, Fresenius J. Anal. Chem. 339. 444-447 (1991)

The hydrolysis of clofentazine and related tetrazines as the basis of determination of residues in bovine tissues.

Somerville, L., Meded. Fac. Landbouww. Rijksuniv. Gent, 45, 841-848 (1980)

The analysis of prochloraz residues in cereals

142

Specht (1), W. & Tillkes, M., Fres. Z. Anal. Chem., 307, 257-264 (1981)

Gas-chromatographische Bestimmung von Ruckstanden von Pflanzenbehandlungsmitteln nach Clean-up uber Gel-Chromatographie und Mini-Kieselgel-Soulen-Chromatographie; 4. Mitteilung: Gas-chromatographische Bestimmung von 11 herbiciden Phenoxyalkancarbonsauren und ihren Estern in Pflanzenmaterial

20, 121

Specht (2), S and Tilkes, M, Fres. Z. Anal. Chem., 322, 443-455 (1985)

Gas-chromatographische Bestimrnung von Rỹckstanden von Pflanzenbehandlungsmitteln nach Clean-up uber Gel-Chromatographie und Mini-Kieselgel-Sọulen-Chromatographie, V. Methode zur aufarbeitung von Lebensmitteln und Futtermitteln plantzlicher und tierischer Herkunft fur die bestimmung lipoid und wasserlửslicher Pflanzenbehandlungsmittel.

162

Stan, H.J., Heil, S., Fresenius J. Anal, Chem. 339, 34-39 (1991)

Two dimensional capillary gaschromatography with three selective detectors as a valuable tool in residue analysis-State of the art

191

Stijve (1), T., Deutsche Lebensm. Rundsch., 77, 99-101 (1981)

Gas chromatographic determination of inorganic bromide residues - a simplified procedure

47

Stijve (2), T., IUPAC Pesticide Chemistry, Human Welfare and the Environment, J. Miyamoto (edit.), Pergamon Press, Oxford, UK, 95-100 (1983)

Miniaturised methods for monitoring organochlorine pesticide residues in milk

1, 21, 43, 44, 48, 71

Stijve (3), T. & Brand, E., Deutsche Lebensm. Rundsch., 73, 41-43 (1977)

A rapid, low cost, small-scale clean-up method for the determination of organochlorine pesticide residues in fats and oils

1, 12, 21, 43, 44, 48

Stijve (4), T., Deutsche Lebensm. Rundsch., 81, 321-322 (1985)

Inorganic bromide - a simple method for the confirmation of residue identity

47

Stijve (5), T., Deutsche Lebensm. Rundsch., 76, 234-237 (1980)

Thin-layer chromatographic determination of chlormequat residues in various substrates

15

Stijve (6), T., Deutsche Lebensm. Rundsch., 76, 119-122 (1980)

The determination of bromopropylate residues

70

Stijve (7), T., Challenges to Contemporary Dairy Analytical Techniques, Royal Society of Chemistry (London), Publ. no. 49, 293-302 (1984)

Determination and occurrence of organophosphorus pesticide residues in milk

4,14, 17, 18, 19, 22, 25, 27, 28, 34, 37, 49, 60, 86, 90

Tadeo, J.L. et al, J. Chrom. 391. 338-342 (1987)

Determination of fenpropimorph in citrus fruit by reverse phase HPLC

Thornton, J.S., Olsen. T.J. and Wagber, K., Agr. Food Chem. 25, 573-576 (1977)

Determination of residues of metsystox-R and metabolite in Plant and animal tissue and soil

164

Tjan, G.H. & Konter, Th., JAOAC, 54, 1122-1123 (1971)

Gas-liquid chromatography of Morestan residues in plants

80

Tuinstra, L.G.M.Th. & Kienhuis, P.G.M., Chromatographia, 24, 696-700 (1987)

Automated two-dimensional HPLC residue procedure for glyphosate on cereals and vegetables With postcolumn fluoregenic labelling

158

VanHaver, W., Z. Lebensm. Unters. Forsch., 172, 1-3 (1981)

Determination of carbendazim and thiophanate-metylresidues in some vegetables and fruits by highpressure liquid chromatography

72, 77

VanWees, A.M.P. et al., in: Chromatography and Mass Spectrometry in Nutrition Science and Food Safety, A.Frigerio & H. Milon (edits.), Elsevier, Amsterdam, Netherlands, 19-25 A(1984)

Chromatographic methods for the determination of inorganic bromide in vegetables

47

Veierov, D. & Aharonson, N., JAOAC, 63. 532-535 (1980)

Economic method for analysis of fluid milk for organochlorine residues at the 10 ppb level 1 (not applicable to dieldrin), 12, 21, 43, 44, 48

Vuik, J. J. Chromatogr. 553 299-304 (1991)

Rapid determination of abamectin in letluce and cucumber by high-performance liquid chromatography.

177

Wagner, K. and Thomton, J.S. Pflanzensch. Nachr. Bayer, 30 1-17 (1977)

Method for the gas-chromatographic determination of metasystox(i) and Metasystox R residues in plants, soil and water (German edit.: 30, 1-17 (1977)

73, 164, 166

Westcott. N.D., J Environm. Science and Health 323, 317-330 (1988).

Terbufos residues in wheat and barley.

167

Wigfield, Y.Y. and Lanquette, M. JAOAC, 74. No.5. 842-847 (1991)

Rcsidue analysis of glyphosate and its principal metabolite in certain cereals, oilseeds and pulses by liquid chromatography and post-column fluorescence detection.

158

Winell, B., Analyst, 101, 883-886 (1976)

Quantitative determination of ethoxyquin in apples by gas chromatography

35

Wright, D., JAOAC 70, 718-720 (1987)

New method for the determination of 1,1-dimethylhydrazine residues in apples and peaches

104

Yamada. T. et al., Agric. Biol. Chem., 48. 1883-1885 (1984)

Determination of residual thiabendazole in citrus fruits and bananas by high performance liquid chromatography

65

Zimmerli, B. & Marek, B., Mitt. Geb. Lebensm. Unters. Hyg., 63, 273-289 (1972)

Entwicklung einer gaschromatographischen Bestimmungs- und Bestatigungsmethode fur Hexachlorbenzolrỹckstọnde in Fetten und Oelen

44

Van Zoonen, P., E.A. Hogendoorn, D.C. van Harten, Meded. Fac. Landbouwwetenschappen Rijksuniversiteit Gent, 55 (3b), 1285-1290 (1990)

Determination of tenpropimorph residues in grains by LC followed by confirmation by GC-MPD.

188