report of visit to the bureau of cosmetics and hazardous substances

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REPORT OF VISIT TO THE BUREAU OF COSMETICS AND HAZARDOUS
SUBSTANCES OF THAILAND, 4-6 DECEMBER 2012
TABLE OF CONTENTS
Page
1.
INTRODUCTION
2
2.
OBJECTIVES OF THE VISIT
2
3.
METHOD OF WORK
2
4.
INSTITUTIONAL CAPACITY
3
4.1
4.2
4.3
4.4
4.5
3
4
5
5
6
Organization and management
Documentation
Laboratory facilities, equipment and materials
Human resources
Laboratory procedures
5.
CONCLUSIONS AND RECOMMENDATIONS
6
6.
PROPOSED ACTION PLAN
7
7.
ACKNOWLEDGMENTS
7
ANNEX 1.
ANNEX 2.
LIST OF MAIN EQUIPMENT OF THE BUREAU FOR QUALITY
CONTROL OF PESTICIDES
8
STAFF OF THE BUREAU OF COSMETICS AND HAZARDOUS
SUBSTANCES THAT ARE INVOLVED IN PESTICIDE-RELATED WORK
AND THEIR QUALIFICATIONS.
11
ANNEX 3.
SCOPE OF ACCREDITATION
13
ANNEX 4.
LIST OF VALIDATED METHODS FOR ANALYSIS OF PESTICIDES
15
1
1.
INTRODUCTION
The use of sub-standard public health pesticide products can have serious adverse effects
on human health and the environment. It can also result in not only ineffective public health
pest or vector control operations, thus leading to increasing application rates and cost, but
also loss of human lives. It may increase the risk to users and the environment as substandard formulations may contain impurities which can increase the toxicity of the product
to mammals and other non-target species. Noting the limited capacity of Member States in
quality control of public health pesticides, designation of regional laboratories that can assist
national programmes and other stakeholders in quality control of public health pesticides is
of prime importance and of high priority.
In Thailand, pesticides are regulated under the Hazardous Substances Act, B.E. 2535
(1992) (3rd Amendment, 2008). It is an umbrella Act that controls pesticides as well as other
hazardous substances, e.g. radioactive substances and disinfectants.
The regulations involving registration and licensing of pesticides are under purview of four
department/agencies in Thailand, i.e. public health pesticides under the Thai Food and Drug
Administration (FDA) while agricultural pesticides are under the Department of Agriculture
(DOA), livestock pesticides are under the Department of Livestock Development (DLD) and
pesticides used in fisheries are under the Department of Fisheries (DOF).
Quality control of pesticides is conducted by different laboratories based on their area
(sector) of use. The Bureau of Cosmetics and Hazardous Substances of the Department of
Medical Sciences (DMSc) is the designated national reference laboratory for quality control
of public health pesticides. Established in 1987, the Bureau supports enforcement of
pesticide regulations and cooperates with the Thai FDA.
2.
OBJECTIVES OF THE VISIT
The objective of the visit was to assess the capacity of the Bureau of Cosmetics and
Hazardous Substances of the Department of Medical Sciences, Ministry of Public Health,
Thialand for quality control of public health pesticides and its potential for designation as a
WHO Collaborating Centre.
3.
METHOD OF WORK
Dr Morteza Zaim, Coordinator, Vector Ecology and Management Unit of the World Health
Organization (WHO) Department of Control of Neglected Tropical Diseases, and Dr Olivier
Pigeon (Head of the WHO Collaborating Centre for Quality Control of Pesticides - CRA-W,
Belgium), WHO Temporary Adviser, visited the Bureau of Cosmetics and Hazardous
Substances, in Bangkok, from 4 to 6 December 2012.
The assessment of the capacity included interviews and discussions with the Director of the
Bureau, Ms Chaivanit Hansa, and with Ms Anantasinkul Nawaporn, Senior Medical Scientist
and MS Siriwat Kultida , Risk Assessment Section Chief, Quality manager as well as other
staff involved in quality control of pesticides. The assessment also included visit to the
laboratory and other relevant facilities of the Bureau as well as direct observation and critical
review of the organization and management of laboratory procedures. Dr Popattanachi
2
Niphon, Director-General of the Department of Medical Sciences was briefed on the mission
objectives and observations.
4.
INSTITUTIONAL CAPACITY
4.1
Organization and management
The Bureau of Cosmetics and Hazardous Substances is one of the twenty-four
bureaus/institutes/regional centres of the Department of Medical Sciences, located in the
campus of the Ministry of Public Health in Muang District, Nonthaburi, Thailand. The Bureau
is composed of four technical Sections (Quality and Technical Development; Risk
Assessment; Quality and Safety Testing; and Standard Methods) and an administrative
section, as presented in Figure 1. Ms Chaivanit Hansa, Director of the Bureau, is supported
by a Senior Medical Scientist and four Section Chiefs. Ms Chaivanit has assumed the post of
the Director of the Bureau since 2007.
Figure 1. Organogram of the Bureau of Cosmetics and Hazardous Substances
(December 2012)
DIRECTOR-GENERAL (Dr P. Niphon)
DEPARTMENT OF MEDICAL SCIENCES
Deputy Director-General (Ms B. Juripom)
Director (Ms H. Chaivanit)
Bureau of Cosmetics and Hazardous Substances
Senior Medical Scientist (Ms A. Nawaporn)
Administrative
Quality and
Technical
Development
Standard Method
Risk Assessment
Quality and Safety
Testing
The activities of the four technical Sections are briefly as follows:
o
o
o
o
Quality and Technical Development – development and maintenance of quality
management system; conduct of proficiency testing.
Risk Assessment – assessments for improving regulation of cosmetics and
hazardous substances; development and evaluation of test kits in cosmetics and
hazardous substances.
Quality and Safety Testing – testing quality, safety and efficacy of cosmetics and
hazardous substances for conformity to standards.
Standard Method – development and validation of test methods; conducting training
on test procedures.
The Bureau of Cosmetics and Hazardous Substances serves as the national reference
laboratory for research and development in cosmetics and hazardous substances, including
3
public health pesticides, in accordance with the Cosmetics Act 1992 and the Hazardous
Substances Acts 1992 and 2008.
The Bureau has established the quality management in the laboratories since 1992 and has
been accredited according to ISO/IEC 17025 by the National Association of Testing
Authorities of Australia (NATA) in medical devices testing in 1995. The scope of
accreditation has been extended to hazardous substances and cosmetics testing. The
Bureau has been also granted from accreditation body in Thailand, i.e., the Bureau of
Laboratory Quality Standards (BLQS).
The Bureau is mainly funded by the government (90% of the budget). Additional resources
come from standard fees charged to manufacturers (10% of the budget) for the analysis of
their products. The staff salaries are paid by the government.
4.2
Documentation
The Bureau has set up a very good and detailed documentation system. A quality manual is
available to describe the management of the laboratory according to the requirements of the
ISO/IEC 17025 standard and of the accreditation bodies (NATA and BLQS). Standard
Operating Procedures (SOP), work instructions and worksheets are available for the
following activities: management, safety, waste treatment, test methods, calibration,
reference materials and reference cultures, instruments and equipment, sample handling,
cleaning, reagent / media preparation, standard solutions, training, audit, proficiency tests,
method validation and verification and sample preparation.
The Bureau has SOPs to guarantee the impartiality and prevention of conflict of interest and
to protect the customer’s confidentiality and proprietary rights. The documents are prepared,
reviewed and approved according to a well-established SOP. Testing service submission
forms serve as contracts between the Bureau and customers before starting the analysis.
The Bureau has SOPs for the resolution of complaints, corrective actions of nonconforming
work and for preventive actions. The training of the staff is recorded in standard forms.
Testing methods are fully described in SOPs. The Bureau has developed and validated
analytical methods for 61 pesticides. These pesticides are those registered in Thailand for
public health uses. The main methods for determination of active ingredient in pesticides
are in-house validated methods. The analytical methods of the Collaborative International
Pesticide Analytical Council (CIPAC) are used for some insecticides, namely allethrin
isomers, deltamethrin, permethrin, piperonil butoxide, pyrethrins, temephos and
cypermethrin. The Bureau plans to implement further CIPAC methods in the future.
The test reports with raw data are archived for a period of at least 10 years after completion
of the testing. After completion of the testing, the pesticide samples are stored as followings:




samples submitted by government sectors ,exclusion of court case , and conform to
the regulation, storage time of three months.
samples submitted by government sectors and not conformed to the regulation,
storage time of one year.
samples for court case , store for at least ten years or until the course case end.
samples submitted by private sectors, could be returned to the submittor or stored for
one month.
There is however no established system for collection and safe disposal of pesticide
samples at the end of this period.
4
The Bureau conducts annual management reviews. The reviews take account of the
following issues: suitability of policy and procedures, reports from section chiefs and
laboratory supervisors, outcome of recent internal audits, corrective and preventive actions
to improve quality of work, assessments from accreditation bodies, results of inter-laboratory
comparisons, changes in the volume and type of work, results of customer satisfactory
evaluations, complaints, recommendations for improvements, quality control of testing,
resources such as personnel, equipment, needed convenient accessories and staff training.
The Bureau performs also internal audits every year.
4.3
Laboratory facilities, equipment and materials
The Bureau has all the necessary facilities and locals for receipt and preparation of pesticide
samples as well as for their analysis. The Bureau also has all the materials (e.g. analytical
standards and solvents) and equipment required to determine the active ingredient content
and impurities in a pesticide product. However their experience has been limited to the
determination of the former only. The main equipment of the Bureau for quality control of
pesticides is listed in Annex 1. This includes gas chromatographs equipped with
autosamplers and different detectors, flame ionization detectors (FID), electron capture
detectors (ECD), mass spectrometry detectors (MS), nitrogen chemi-luminescence detector
(NCD) and high-performance liquid chromatographs equipped with autosamplers and UV
diode-array spectrometry detectors (DAD).
The Bureau have some equipment to assess physical parameters of common public health
pesticide formulations for some parameters, namely pH range, suspensibility, persistent
foam, wettability, wet sieve test , emulsion characteristic and re-emulsion and water content
(Karl Fischer method). However some equipment and materials are required to assess
other chemical properties as well as physical parameters of common public health pesticide
formulations. Such analysis is critical to safety and good performance of a pesticide
formulation.
All laboratories are equipped with appropriate working tables, fume hoods and ventilation
systems. Most laboratories are equipped with air-conditioning. Locals for sample preparation
and storage however need to be equipped with air-conditioning. The locals for storage of
pesticide samples and solvents should be better ventilated and better secured against fire
and for other safety aspects.
The local for archiving of documentation and reports of the Bureau should be extended and
properly secured, including against fire.
4.4
Human resources
The list of the staff of the Bureau and their experience and qualifications is presented in
Annex 2. The staff are well-trained for determination of active ingredient content in pesticide
products. They however require further trainings on testing chemical and physical
parameters of pesticides and in use of CIPAC methods. The motivation of staff in performing
their duties was notable.
5
4.5
Laboratory procedures
The main activities of the Bureau are focused on the analysis of cosmetics, disinfectants and
pesticides. The Bureau is responsible for the chemical and microbiological testing of public
health pesticides according to the Hazardous Substances Act. Chemical testing covers the
active ingredient content in the formulated pesticide products. About 700 pesticide samples
are analysed annually for active ingredient content. Average time for analysis and reporting
is about one month. The Bureau does not sub-contract any testing. The source of samples
analysed are mainly from the Thai FDA, in the framework of surveillance programmes, and
also from pesticide manufacturers.
The Bureau has in place appropriate standard operating procedures and manuals for
receipt, registration, handing and analysis of pesticide samples. The sample preparation and
their chromatographic analysis are performed according to well described analytical
methods. However many such methods are in-house and not methods specified by WHO
specifications (e.g. CIPAC) for wide acceptance. The list of analytical methods accredited
according to ISO/IEC 17025 is given in Annex 3. Many analytical methods used by the
Bureau for quality control of pesticides are validated for their linearity, precision, accuracy,
and where relevant, their limit of detection and quantification. However validation has not
been performed for all the methods used by the Bureau for quality control of pesticides and
need to be addressed. The list of validated analytical methods for the analysis of pesticides
is given in Annex 4.
All major equipment are routinely calibrated in-house and or by external agents. Records of
maintenance and calibration are available. In addition all laboratory operations are recorded
in appropriate work sheets. All pesticide samples, analysis and reporting are identified by a
unique bar code. There is however room for further computerization of the information/data
throughout their chain of custody.
Quality and accuracy of data is properly verified through appropriate laboratory measures
including duplicate injections and analysis, analysis of blanks, check calibration solutions
and spiked samples. The Bureau has participated in recent CIPAC collaborative trials of
chlorfenapyr and piperonyl butoxide and has organized a national proficiency test on
temephos granules in their attempts to further improve analysis of pesticides.
5.
CONCLUSIONS AND RECOMMENDATIONS
The Assessment Team has noted the excellent capacity of the staff of the Bureau of
Cosmetics and Hazardous Substances in pesticide analytical methods and laboratory
practices. The Team also noted the good procedures and practices in place to ensure
quality of analysis and documentation.
Quality control of pesticides by the Bureau, however, is largely limited to the determination of
active ingredient which is not sufficient for full assessment of quality of pesticide products for
their safety and good performance.
In order to fulfil the two-year probationary period of satisfactory collaboration between the
Bureau and WHO, which is a requirement for designation as a WHO Collaborating Centre,
the following activities and actions are recommended:
6
o
strengthen the capacity of the Bureau for testing of all physical and chemical properties
of a public health pesticide product, including relevant impurities, as specified in the
WHO specifications and as part of its quality control; promote and support conduct of
such full testing as a policy for national regulation of public health pesticides;
o
use collaboratively tested analytical and other test methods as specified by WHO
specifications (e.g. CIPAC), to ensure wide acceptability and application of results of
quality assessment of public health pesticide;
o
Continue participation in proficiency tests and collaborative studies of international
organizations, such as CIPAC, as a strategy for further strengthening the capacity of the
Bureau for quality control of public health pesticides; and
6.
PROPOSED ACTION PLAN
1. Develop, based on WHO specifications for public health pesticides (PHPs), the list of
physical and chemical parameters and methods of analysis;
2. Develop the list and acquire materials and equipment required to perform the full
physical and chemical testing of PHPs according to WHO specifications;
3. Acquire expertise on the conduct of physical and chemical analysis of public health
pesticide products, including long-lasting insecticidal nets;
a. Train 2 scientists/technicians in the WHO Collaborating Centre for Quality Control
of Pesticides, Gembloux, Belgium;
b. Conduct inter-laboratory comparison studies on selected physical and chemical
tests between the Bureau and the above-mentioned WHO Collaborating Centre;
c. Participate in CIPAC organized collaborative trials for pesticides; attend annual
CIPAC Technical Meetings;
4. Organize visit of the Bureau by a WHO expert to assess implementation of physical
and chemical testing of PHPs
5. Develop and submit to WHO a full report on implemented activities within the
probationary period.
7.
ACKNOWLEDGEMENTS
The WHO Assessment Team wishes to thank the Director and the staff of the Bureau of
Cosmetics and Hazardous Substances of the Department of Medical Sciences for their
interest in and for their commitment to the work of WHO, and for their collaboration and
support of this assessment.
7
ANNEX 1.
LIST OF MAIN EQUIPMENT OF THE BUREAU FOR QUALITY CONTROL
OF PESTICIDES
No.
Equipment
Products / Models
1
Automatic titrator
Metrohm / 702SM
2
Automatic titrator
Metrohm / 751 Titrino
3
Automatic titrator
Metrohm / 907 Titrino
4
Balance, electronic precision
( 0.001 g )
Precisa / XT 1220M
5
Balance, electronic analytical
( 0.0001 g )
Mettler / AT 200
5
Balance, electronic analytical
( 0.0001 g )
Sartorius / LA 230S
6
Balance, electronic analytical
( 0.0001 - 0.00001 g )
Mettler / AX 105 DR
7
Balance, electronic analytical
( 0.0001 - 0.00001 g )
Mettler / XP 205 DR
8
Bath, Cooling with external circulator
LAUDA / E 100
9
Bath, Water with temperature control
Memmert / EB 29
10
Deionizer
Millipore / Milli-Q Plus 185
11
Deionizer, Mixed Bed
Yamato / Autosil WA53-2
12
Deionizer, Mixed Bed
Barnstead / D7033
13
Densitometer, TLC Scanner
CAMAG / Scanner 3
14
Flashpoint tester
SETAHOPE / SETAFLASH
15
Fume hood
Easy lab / 200
16
Fume hood
Easy lab / 200
17
Fume hood
Easy lab / 150
18
Fume hood
Easy lab / 200
19
Fume hood
Easy lab / 150
20
Fume hood
Easy lab / 150
21
Fume hood
Easy lab / 150
8
22
Fume hood, Walk in
Easy lab / 200
23
Fume hood, Walk in
Easy lab / 200
24
Fume hood, Walk in
Easy lab / 200
25
Gas Chromatograph (GC)
Agilent / 6890N
26
Gas Chromatograph (GC)
Agilent / 6890N
27
Gas Chromatograph (GC)
Agilent / 7890 A
28
Gas Chromatograph (GC)
Agilent / 7890 A
29
Gas Chromatograph (GC)
Agilent / 7890 A
30
Gas Chromatograph-Mass Spectrometer (GCMS)
Agilent / 6890N
31
HPLC
WATERS
32
HPLC
WATERS
33
HPLC
WATERS
34
HPLC
WATERS
35
HPLC
WATERS / e2695
36
HPLC
WATERS / e2695
37
LC/MS/MS
WATERS / XEVO TQ-S
38
Incubator, aerobic
WTB Binder / BED-115
39
Ion analyzer
ORION / 930
40
Ion Chromatograph
DIONEX/ICS-3000 series
41
Melting point Apparatus
OPTIMELT / MPA 100
42
Oven , hot air
WTB Binder / ED 531E
43
Oven , hot air
Termaks / TS 8136
44
Polarimeter
KRUSS / P 8000-T
45
Reference, weight (22 pieces)
Masscal / F1
46
Reference, weight
SARTORIUS / E2 (1 g)
47
Reference, weight
SARTORIUS / E2 (10 g)
9
48
Reference, weight
SARTORIUS / E2 (50 g)
49
Reference, weight
SARTORIUS / E2 (100 g)
50
Reference, weight
SARTORIUS / E2 (200 g)
51
Reference, weight
LS/F1(2150207-1-1)(500 g)
52
Reference, weight
LS/F1(2150207-2-1)(500 g)
53
Reference, weight (23 pieces)
Hafner / E2
54
Refractometer, reflactive index
KRUSS / DR 6100-T
55
Refrigerated centrifuge high speed
(up to 26,000 rpm)
Thermo / IEC B-22 M
56
Refrigerator
Sanyo / SR-F380
57
Refrigerator
Sanyo / SR-NF135
58
Refrigerator
STRONGMAN
59
Refrigerator
STRONGMAN
60
Refrigerator, T
MITSUBISHI / MR-F56C-DS
61
Refrigerator, explosion proof
HOTPACK / 825150
62
Thermometer
PRECISION
63
Thermometer
GOLD BRAND
64
Thermometer, Mercury
Arno Amarell
65
Timer , Stopwatch
Heathrow Scientific / HEA24490M
66
UV-VIS spectrophotometer
SHIMADZU / UV-160A
67
UV-VIS spectrophotometer
PERKIN-ELMER / Lambda 2S
10
ANNEX 2 .
STAFF OF THE BUREAU OF COSMETICS AND HAZARDOUS SUBSTANCES THAT ARE INVOLVED IN PESTICIDERELATED WORK, AND THEIR QUALIFICATIONS.
A. Senior scientists
Name
Anantasinkul Nawaporn
Meesri Junya
Siriwat Kultida
Meethong Sudthida
Tianungoon Suwunna
Degree
MSc.(Statistic); BSc.(Chemistry)
BSc.(Chemistry)
MSc.(Microbiology); BSc.(Biology)
MSc.(Analytical Chemistry); BSc.(Chemistry)
PhD.(Microbiology);MSc.(Toxicology);
BSc.(Biology)
# year
34
23
25
25
23
Section
Senior Medical Scientist
Quality and Technical Development Section Chief
Risk Assessment Section Chief, Quality Manager
Quality and Safety Testing Section Chief
Standard Method Section Chief
B. Junior scientists
Name
Nakniyom Wongdaun
Nilmanee Laweng
Vivon Menaka
Nitchanpansri Jiraporn
Suriyajun Woramon
Chaichana Jatuporn
Sangjarusvichai Haruthai
Intharasamee Kamolluck
Khejonnit Awiruth
Kao-ian Chun-grida
Noppkue Napaputch
Degree
MSc.(Analytical Chemistry); BSc.(Chemistry)
MSc.(Medical Sciences); BSc.(Chemistry)
MSc (Cosmetic Sciences); BSc.(Chemistry)
MSc.(Analytical Chemistry); BSc.(Chemistry)
BSc.(Pharmaceutical Sciences)
MSc.(Analytical Chemistry); BSc.(Chemistry)
MSc.(Analytical Chemistry); BSc.(Chemistry)
BSc.(Chemistry)
BSc.(Chemistry)
BSc.(Pharmaceutical Sciences)
MSc (Cosmetic Sciences); BSc.(Chemistry)
11
# year
20
15
12
3
3
1
1
17
18
2
5
Section
Standard Method Supervisor
Quality and Safety Testing Analyst
Risk Assessment Analyst
Quality and Safety Testing Analyst
Standard Method Analyst
Standard Method Analyst
Quality and Safety Testing Analyst
Quality and Safety Testing Analyst
Risk Assessment Supervisor
Quality and Safety Testing Analyst
Standard Method Analyst
C. Technicians (Temporary Staff, Medical Scientists)
Name
Suwannatrai Wadeelunate
Santa Sumita
Kompayak Preechaya
# year
9
1
1
section
Quality and Safety Testing Analyst
Quality and Safety Testing Analyst
Quality and Safety Testing Analyst
D. Administration officer
Name
Sajjathanasakul Chommanee
Boonyoung Prapaipak
Wongkumjun Panrapeeput
Deeying Jumpa
Injai Jiravadee
# year
1
30
18
25
20
12
section
Administration
Administration Section Chief and
Document Control Officer
Administration Sample Custodian
Administration
Administration Sample Custodian
ANNEX 3.
SCOPE OF ACCREDITATION
National Association of Testing Authorities (NATA), Australia
Accreditation No. 10627 of 08 June 2011
Type of sample
Insecticide and acaricide
formulations including
insecticide treated nets
Mosquito larvicides
Compound
Method
Allethrin
GC, SOP 06-02-264
Alpha-cypermethrin
GC, SOP 06-02-264
Bifenthrin
GC, SOP 06-02-264
Chlorpyrifos
HPLC, SOP 06-02-263
Cyfluthrin
GC, SOP 06-02-264
Cypermethrin
GC, SOP 06-02-264
Deltamethrin
GC, SOP 06-02-151
and SOP 06-02-264
Dichorvos
GC, SOP 06-02-264
Fenvalerate
GC, SOP 06-02-264
Fipronil
HPLC, SOP 06-02-194(T)
Imiprothrin
GC, SOP 06-02-264
Permethrin
GC, SOP 06-02-069
and SOP 06-02-264
Phenothrin
GC, SOP 06-02-264
Piperonyl butoxide
GC, SOP 06-02-264
Prallethrin
GC, SOP 06-02-264
Tetramethrin
GC, SOP 06-02-264
Temephos
Normal phase HPLC,
SOP 06-02-081
Temephos
Reverse phase HPLC,
SOP 06-02-201
13
ANNEX 3 continued. SCOPE OF ACCREDITATION
Bureau of Laboratory Quality Standards (BLQS), Thailand
Accreditation No. 4031/49 of 09 December 2011
Type of sample
Insect repellents
Compound
Method
Citronella
GC, SOP 06-02-122
N,N-diethyl-m-toluamide
HPLC, SOP 06-02-199
Dimethyl phthalate
HPLC, SOP 06-02-199
Ethyl butylacetyl
aminopropionate
HPLC, SOP 06-02-199
N,N-diethyl-m-toluamide
SOP 06-02-050
based on AOAC (2010) 985.03
d-Limonene
HPLC, SOP 06-02-248
Permethrin
SOP 06-02-191
based on AOAC (2010) 991.03
Cypermethrin
SOP 06-02-191
based on AOAC (2010) 991.03
Pet shampoo
Flumethrin
HPLC, SOP 06-02-057
Insecticide chalk
Cypermethrin
SOP 06-02-275
based on AOAC (2010) 991.03
Deltamethrin
SOP 06-02-275
based on AOAC (2010) 991.03
Insecticides
14
ANNEX 4.
LIST OF VALIDATED METHODS FOR ANALYSIS OF PESTICIDES
No
Compound
Technique*
1
2
3
N, N diethyl-m-toluamide
flumethrin
citronellal
GC
HPLC
GC
4
5
6
7
8
9
10
11
12
13
Cypermethrin and permethrin
Insect repellants :dimethyl phthalate , ethyl butylacetyl and N,N-diethyl-m-toluamide
d-limonene
Cypermethrin and deltamethrin
permethrin
temephos
deltamethrin- bed net
fipronil
chlorpyrifos
alphacypermethrin ,bifenthrin, cyfluthrin ,cypermethrin, deltamethrin, dichlorvos, fenvalerale, Imiprothrin, permethrin and
phenothrin
allethrin isomers
HPLC
HPLC
HPLC
HPLC
GC
HPLC
GC
HPLC
HPLC
GC
14
*
GC = gas chromatography; HPLC = high-performance liquid chromatography
15
HPLC and GC
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