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Decontamination of pesticide residues in fruits and vegetables

Preferably, the RAC samples used in the preparation studies to contain measurable treated waste as close as possible to the MRL, so that measurable residues are obtained, and transfer factors different products are processed can be determined. A transfer factor gives the ratio of the concentration of residue in the processed product to FCAC. For example, if the concentration of waste is 0.5 mg / kg of olives and 0.2 mg / kg in olive oil, transfer factor is 0.2/0.5 = 0.4. A factor 1 (= concentration factor) indicates a concentration effect of treatment procedures. Improved waste, either by increasing the application rate, to shorten the pre-harvest interval (PHI) or in vitro nails with RAC and its active metabolites are not generally desirable. Doping is acceptable only if the waste can be demonstrated that the CAR includes only waste the surface. However, PHISO in some cases, especially when waste in the CARs are near the analytical limit of determination of the value field treatment exaggerated or small, it is advisable to obtain levels of residues of sufficient treatment studies.

The first step in the home or food processing business is the preparation food using a series of mechanical processes, such as removing damaged or dirty or parts of plants, washing, peeling, peeling or shelling. This often leads to a significant reduction in the amount of pesticide residues in other edible parts (Petersen et al. 1996; Celik et al. 1995; Schattenberg et al., 1996).

WASHING

Household cleaning procedures are generally performed with the operation or standing water at moderate temperatures. Detergents, chlorine or ozone can be added to the wash water to improve effectiveness of the washing procedure (Ong et al., 1996). If necessary, several methods of washing can be accordingly.

The effects depend on physico-chemical pesticides, such as water solubility, volatility of hydrolysis rate constant, and octanol-water (Pow), compared to the actual physical location of waste washing lead to a reduction in waste that are hydrophilic on the surface of cultures. In addition, the temperature of the wash water and washing has an influence on the level of residues. As noted by Holland et al. (1994), washing Hot and adding detergents are more effective than cold water washing. Wash with rubbing gently by hand with water tap water for 1 min remove pesticide residues significantly (Barooah and Yein, 1996). Systemic and lipophilic pesticide residues are not removed significantly to wash.

Table (1) shows examples of the effect of washing on levels of pesticide residues in fruits and vegetables.

PEELING

The outer leaves of vegetables often contain residues of pesticides applied during the growing season. Therefore, peeling or cutting procedures reduce residue levels in green leafy vegetables. Peeling roots, tubers and vegetables bulb with a knife is a common practice at home. Many examples show that most of the residues is equal or on the skin. Peeling the CCR may eliminate more than 50% of pesticide residues in commodities. Therefore, the removal of the shell is almost total elimination of waste, leaving little in the edible parts. This is particularly important for fruits that are eaten in the shell, such as bananas or citrus fruits. Reynolds (1996) showed that the peel carrots or cut waste reduction chlorfenvinphos, primiphos-methyl, quinalphos triazophos producing a transfer coefficient of 0.2. However, the skin peeling of business processes can be used as animal food or for the production of essential oils (citrus) or pectin (citrus, apples, etc.). For these industrial processes, it is important to note that, especially in non-systemic residues often focus on shell. For systemic pesticides, the scale may not be as effective as shown Sheikhorgan et al (1994). After applying cucumber thiometon without reducing the level of waste can be detected in the peeled cucumber.

Under the Codex Alimentarius, as in other international standards for MRLs whole fruit, which is appropriate to assess compliance with good agricultural practices. These MRLs are limited reviews, however, to assess dietary exposure to pesticides from fresh fruits, peeling (Holland et al., 1994).

KITCHEN

Kitchens and procedures at different temperatures, the duration of the process, the amount of water or food additives, and system type (open or closed) may have an impact on waste levels. Generally, waste is reduced during the cooking process by volatilization in open systems hydrolysis or closed systems. In all cases, the liquid also dilutes the kitchen waste. Several studies have been reported in the dissipation of pesticides on crops during cooking. In addition to the studies summarized in Table 1, the behavior of organophosphorus pesticides chlorfenvinphos, fenitrpothion, isoxathion, methidathion and prothiophos during cooking has been reviewed by Nagayama (1996) green tea leaves, spinach and fruits. These pesticides have decreased during the process of cooking time to boil. According to its solubility in water, some pesticides moves the materials in water cooking. In addition, the pesticide remains in processed foods based on their octanol-water partition coefficient, which is an indicator of hydrophilic properties or lipophilic molecule. In exceptional cases, the cooking process can cause degradation of pesticides giving a reaction product of importance toxicology. For example, degrades daminozide DMH (1, 1-dimethylhydrazine), which is much more potent than the parent compound (Leparulo-Lofus et al., 1992). Another example is the formation of ETU (ethylene thiourea) of EBDC (ethylene bisdithiocarbamate) fungicides such as mancozeb, during heating process (Petersen et al., 1996).

Immersion in a chemical solution

solution of sodium chloride, are widely used to decontaminate waste pesticides in various fruits and vegetables. There are several studies to test the effectiveness of salt water wash to remove pesticides cultures. In this process, the sample chopped fruit and vegetables are placed in a beaker containing 5% solution of sodium chloride. After 15 minutes, samples of plants were rubbed gently with your hand solution of salt and water is decanted alt. Examples of the effect treatment with saline in the levels of pesticide residues that are applied to different plants are shown in Table 1.

Kumar et al (2000) reported that the dumping of green peppers in a 2% saline for 10 minutes followed by washing with water is effective in facilitating the elimination of 32.56 and 84.21% for residues at 0 and 5 days of the application triazophos (700 g ai / ha), while residues of acephate were taken to an area of 78.95% to zero days. Following the same technique of Kumar et al (2000) observed 90.56% reduction in days and66.93 result in 0 and 5 after the spraying of cypermethrin in peppers.

Dip fruit in the treatment of NaCl, HCl, acid, acetic acid, NaOH, potassium permanganate removed 50-60% of the residues on the surface of the synthetic pyrethroids compared 40-50% of Hydrolytic degradation with NaOH (Awasthi, 1986b).

aqueous NaOH, potassium dichromate and acetic acid solution soapy acid used as decontamination agents for Tom ... ... ... ....

Treatment of fruit with tamarind sauce 2% solution for 5 minutes followed by washing with tap water and steam cooking for 10 min. Has been found to eliminate the waste of monocrotophos, carbaryl and fenvalerate to an extent of 41.81, 100 and 100% respectively. The treatment with a salt solution of 2% was equally effective.

Dip eggplant treatments wioth fruit water, sodium chloride, HCl, acetic acid or potassium permanganate solution were found to eliminate all waste 30-33% of fenvalerate, permethrin, deltamethrin and cypermethrin NaOH at 40-45% and teepol (detergent) solution 50-60%. The effect of washing on the reduction of waste has decreased in the second and third crops.

Many experiments have been carried the three common household, namely preparations. washing with water, salt water for washing and cooking in order to evaluate their effectiveness relative reduction of pesticide residues in different plants. The results are summarized in the following table.

Table: effect of washing the salt water for washing and cooking on residue levels of pesticides.

Crop residues of pesticides Results% expelled Reference *

Rinse

Water from the wash water Kitchen

Cauliflower 41-48 Methamidophos 46-47 46.94

-53.54 Largest decrease was caused by cooking. Jacob and Verma (1990)

Okra

Methamidophos

64-72

19-58

58-64 water washing can remove debris indicating maximum solubility in water, but most of all processes below values TMRL. Jacob and Verma (1990)

Cauliflower alpha-cypermethrin

_ 7-38

12-17 was more effective washing the kitchen probably due to the thermal stability cypermethrin. Malik et al (1997)

Cabbage

Chlorpyrifos

Quinalphos

38

41

52.13

56.50

54.3

55 With all three process waste has been reduced to some extent. They may reduce residues below the MRL. Thus, a waiting period for a minimum of one and two weeks respectively, it was proposed regardless of washing and cooking for chlorpyrifos quinalphos neck. Nagesh and Verma (1997)

cowpea

Metasystox

Carbalyl

84.3

87.5

86.4

88.7

83.4

Only 80.8 cloves boiling samples can detoxify residues within the surface or tissue to the extent of safe limits by the 10th day of treatment. Dikshit et al (1984)

Cauliflower

Malathion

60

70

Cook was 80 to be more efficient and reduces the value TMRL one week to zero days. Jacob and Verma (1989)

Bhindi

Quinalphos

61.84 to 64.35

43-53

78-82

Wash with water and salt water wash residues below the MRL at zero days, the kitchen has also made this up and waste reduction.

Jacob

Verma (1985)

Cabbage

Malathion

Carbaryl

Pyrethroids

64.60

75.40

6.22 (AV)

-

-

-

83.97

89.62

56.72 (average)

The degree of decontamination was higher because of the kitchen from the laundering of all insecticides.

Bhatia and

Verma (1994)

The leaves and dotted with heads of cabbage and cauliflower, the pods of oilseed rape in India

Green beans

Methamidophos

DDT

Malathion

Carbaryl

65.71 to 77.67

71

96

52

-

-

-

-

80 88.88

52 (cooked)

66 (pressure cooked)

99 (cooked)

99 (p.cooked)

77cooked

69 (p.cooked)

Maximum food waste dislodged.

Water washing removes residues of DDT up while the kitchen is effective for removing debris of malathion and carbaryl.

Dikshit et al (1986)

Elkins et al (1968)

The table above may say that the kitchen is more effective in reducing pesticide residues on both different vegetables, but in some cases, washing with water was effective in reducing pesticide residues initial and found that aging waste or increased sampling day of treatment during the washing effect is reduced to eliminate the toxic substance in the same As the samples collected immediately after spraying boiling or cooking, to be effective. One possible reason for removing high percentage of toxic substances in samples collected immediately that most of the residues on the surface of samples and is very easy to remove by simple washing observed by Dikshit et al (1984.86) Elkins et al (1968) Bhatia and Verma (1994) and Malik et al (1998). When wastes are migrating into the deep tissues or strongly adhere to the rough surface of some vegetables. In addition, the washing can not reduce waste at safety with respect to the boil.

There are studies in the three processes mentioned Culinary be effective in reducing residues below the MRL. According to Jacob and Verma (1991) quinalphos residues in crops of cauliflower treaty would be reduced only partially by different processing methods workshop, such as washing and cooking. Nagesh and Verma (1997) suggested that inefficient processes for decontamination of treated cabbage could house because of the strong adsorption properties quinalphos and chlorpyrifos.

Effects of preparation home for the decontamination of pesticides in fruit and vegetables multiresidue

The low levels of pesticide residues were detected in 97 (40%) of 243 meters of additional samples after a normal household washing peeling and cooking procedures. The number of samples containing detectable residues has been reduced to 47 (19%) after the preparation of the house. These results indicate that the level of residues in Most commodities fell substantially after the preparation of the house (Schattenberg et al, 1996).

Ramesh and Balasubramanian (1999) conducted a study with fruit and vegetables collected from local markets Chennai and fortified with known concentrations of various pesticides followed by decontamination study of how different household, such as washing, cooking, peel the 65-95% from the decontamination of pesticide residues in the different steps of 512 samples analyzed raw market, organochlorines and organophosphates in the 12 samples were withdrawn waste to far below the limits of toxicological acceptable.

Rinsing with tap water reduces pesticide residues in short many types of products (Krol et al., 2000). Rinsing removes residues of nine of the twelve pesticides studied. Among captan, chlorothalonil, iprodione, vinclozolin, endosulfan, permethrin, methoxichlor, malathion, diazinon, chlorpyrifos, bifenthrin and DDE residues of vinclozolin, bifenthrin and chlorpyrifos were not removed. This study confirms that the water solubility of pesticides does not play an important role in reducing observed. The majority of pesticide residues on the surface seems to be the products of which are eliminated by the mechanical action washing.

The first studies the effects of the commercial preparation and the house on pesticide residues in fruits and vegetables were summarized by Zabik (1987). Early studies have shown reduced waste to be significant, with a percentage reduction of hydrocarbons chlorinated range of 50-99% + for the commercial preparation and 14-99 +% for the preparation of the house with the exception of parathion in spinach and broccoli, and commercvial Home prewparation substantially reduced organophosphate pesticide residues, the overall reduction, be in the top 80 or 90% of the beach. carbamate residues were reduced by 58-99% + when plants are treated in the trade, but only 11-92% being home preparation.

A recent study in Korea supports these previous studies (Lee and Lee, 1997). They found that 45% of waste is disposed of when food organophosphates washed with water, 56% of detergent washing, peeling with 91% and 51% with bleaching.

Methods of analysis of pesticide residues in fruits and many vegetables

Analysis by gas chromatography

Nakamura et al (1994) developed a method for the analysis of multiple residues of 48 pesticides (20 organophosphate, organochlorine 7, 14 and 7 organonitrogen pyrethroid pesticides) has enabled Japan on the basis of capillary gas after removing pesticides in samples nacetone vegetable and fruit crops or acetonitrile containing lipids backwash followed by ethyl acetate (Solution test). organophosphorus pesticides were directly determined by GC-FPD. Organonitrogen pesticides were determined by GC-FTD (GC-NPD), after cleaning by chromatography silica gel. Organochlorine and pyrethroid pesticides were measured by GC-ECD after cleaning by Florisil column chromatography. The recovery of crops in ten fortification levels from 0.05 to 0.25 ppm were 42.5 to 128.5%. detection limits was 0.001 ppm for organophosphates and organochlorine pesticides and 0.01 ppm for organonitrogen pesticides and pyrethroids.

A method Multiresidue has been used by DEJONCKHEERE et al (1996) for the determination of organochlorine compounds, organophosphorus pesticides and organonitrogen in fruits and vegetables were extracted with acetone followed by liquid-liquid partitioning with water: pesticides in the ether apolar oil phase, polar pesticides extracted from the aqueous layer with dichloromethane and analyzed by gas chromatography with electron capture (GC-ECD), flame photometry (GC-FPD) and thermo-specific detection (GC-TSD).

The method used for determining residues multiple of 52 organophosphate pesticides, including organochlorines, organonitrogen, pyrethroids pesticides and dithiocarbamates certain fruit and vegetables has been described by Dogheim et al (1999) by gas chromatography. The samples were extracted with acetone followed by a partition with hexane and dichloromethane and estimated by GC-ECD and GC-NPD. Dithiocarbamates were digested with a mixture of concentrated HCl, SnCl2 and water for the course of CS2 is in an ethanol solution of copper acetate and diethanolamine to form a yellow complex. Density the yellow product was measured spectrophotometrically at 435 nm. The average recoveries and CV of the 52 pesticides were 72-118 and 1-20%, respectively, levels of more than 0.01 to 1 ppm. A similar method has also been described by Kole et al (1998).

Krol et al (2000) used a multi-residue procedure for the determination of 12 pesticides in vegetables in the samples were extracted with 2 propanol and ether oil followed by washing with distilled water 3 times. The final analysis of the samples was performed by GC-ECD, FPD, XSD and Or ELCD.

Ramesah and Balasubramanian (1999) describes a method of determining organochlorine and organophosphorus pesticides organonitrogen in fruits and vegetables after extraction with 2-propanol and petroleum ether by mechanical shaker followed by distilled water column Partitioning Florisil clean organized crime and organophosphate pesticides. For organonitrogen pesticides was extracted with acetone followed by partitioning with 10% NaCl and ethyl acetate and column cleanup on silica gel. organochlorines, organophosphorus compounds and organic nitrogen were analyzed by GC-ECD, GC-FPD and GC-NPD, respectively.

By GC-ECD, efficiency acetonitrile and acetone to remove the 8 pyrethroids 6 fruit and vegetable samples were compared by Pang et al (1997). The efficiency of extraction acetone has been competing with acetonitrile for the fruit of six samples of vegetables. robustness tests also demonstrated that the method proposed is simple and accurate with good precision and adequate for the analysis of multiple residues of pyrethroids in various agricultural products.

Organophosphate and organochlorine pesticide residues from fruit and vegetables capillary GC with electron capture detector (ECD) nitrogen-phosphorus detector (NPD), flame photometric detector (FPD) of sulfur and phosphorus mode and a mass spectrometric detector (MSD) in monitoring of specific ions (SIM) were determined by the method of Torres et al (1995), after solid phase extraction grid-dispersion (MSPD) has resulted in the recovery of 41-108% with relative SD of 14.2% in conc. range of 0.5 to 10 mg / liter in oranges, lemons, grapefruits, pears, plums, lettuce and tomatoes.

A multiresidue method as described by Sannino et al (1995) for the quantitative determination of organophosphorus 39 (Pesticide Parent and its major metabolites) in 7 fatty processed foods based on gel permeation chromatography with automated column biobeads SX3 and methylene chloride-cyclohexane (15 + 85) eluate after extraction with methylene chloride. organophosphates are quantified by GC-FPD with OV-1701 and DB-5 columns. Average Recovery from spiked samples in 0025-1 mg / kg was 50.6% for dichlorvos to 185% for malaoxon. Determination limits were between 0.005 and 0.040 mug / ML. The results were confirmed by chromatography gas chromatography / mass spectrometry with selected ion monitoring.

Gas chromatography conditions for separation and identification compounds were selected using two capillary columns of different polarities and two detectors, ECD and multiresidue determination NDP amount of 37 pesticides in fruits and vegetables and to study the effectiveness of the gel permeation chromatography clean-up after withdrawal ethyl acetate (Balinova, 1999).

Trova et al (1999) has liquid chromatographic determination of pesticide residues (Including azinphos-ethyl, azinphos-methyl, carbaryl, diflubenzuron dinocap teflubenzuron, and) in vegetables after solvent extraction acetate ethyl n-hexane system methylene chloride, instead of wide. Recoveries as required by the "Guidelines for the control of waste in the European Union have been observed, the solvency of the new system can be considered as an alternative to compounds halogenated hazardous to their toxicity and harmful behavior in the environment in the extraction of active compounds HPLC-determined.

A detection method was proposed by broad Gelsomino et al (1997) for multi-residue analysis of 77 pesticides (organo 12, 45 organonitrogens, September 11 organophosphates and pyrethroids) in agricultural products by gas chromatography equipped with long, narrow-gauge fused silica open open tubular columns and an electron capture detector (ECD). The residues were extracted with acetone followed by dichloromethane and partitioning cleaning gel permeation chromatography. Recoveries of most pesticides from spiked samples of carrot, melon and tomato at fortification levels from 0.04 to 0.10 mg / kg 70-108%. Limits of detection were below 0.01 mg / kg for infants.

Beena et al (2002, 2003) carried out an inspection of samples of plants forming a multiresidue analytical technique using GC-ECD and GC-NPD systems with capillary columns.

Ueno et al (2003) studied a multi-residue method effective and reliable for the determination of Nitrogen-52 and / or phosphorus-containing pesticide residues in many samples of plants from which samples were extracted with acetonitrile and the acetonitrile layer separated was purified by gel chromatography effluent is split into two fractoions pesticides, fractions pesticides were purified, respectively, by a two-step minicolumn cleanup, the fraction of a silica gel minicolumn second to first Tandem fraction minicolumn (florisil minicolumn inserted in silica gel minicolumn) that was elected to the petroleum ether-acetone (3 +7). The combined eluate was subjected to gas chromatography with double column with nitrogen-phosphorus and flame photometric detection. Recoveries 52 pesticides in spiked samples ranged from 72-108% in relation to the standard deviations of 2.17%, except for the recoveries of methamidophos and chorothalonil. The detection limits of pesticides were satisfactory (0001-0009 mg / kg) for the control of pesticide residues in vegetables.

Menkissoglu et al (2004) A study of the effect of the matrix induced by 16 common pesticides, more frequent monitoring studies of the tomato and chilli cucumber, using a simple multiresidue method with GC-ECD or NPD, without prior cleaning step. GC responses abnormally high and very high recoveries for various pesticides in the extracts were obtained by calibration with a standard solution of pesticide ethyl acetate.

A faster, less efficient, more environmentally friendly extraction fluid supercritical (SFE) has been evaluated by the method Garcia et al (1996) compared the methods conventional mining to extract sonvent imidacloprid, methiocarb, chlorpyrifos, chlorothalonil, endosulfan-1, endosulfan sulfate-2 and endosulfan, peppers and tomato plants sample: anhydrous magnesium sulphate (5:7) mixtures perform the extraction with supercritical CO2 HPLC / DAD, GC / ECD and GC FPD / for analysis. The conditions were chosen SFE 300 atm, 500C, 200? The static modifier of methanol, a few minutes time static and dynamic extraction with 15 ml of CO2 and the collection in 3 ml of ethyl acetate. Except for imidacloprid, which has not found in any of the conditions analyzed, recoveries of pesticides were more than 80%.

A simplified method is described by Chaput (1987) reversed-phase liquid chromatography was used post-column derivatization and fluorescence detector to determine 7 N-methyl carbamates (aldicarb, carbaryl, carbofuran, methiocarb, methomyl, oxamyl and propoxur) and 3 related metabolites in fruits and vegetables after the sample extraction with methanol, followed by gel chromatography (GPC) or GPC nuclear Online celite clean crops high chlorophyll and / or carotenoid (eg, cabbage and broccoli). Recovery data were obtained by fortifying Five different crops (apples, broccoli, cabbage, cauliflower and potatoes) at 0.05 and 0.5 ppm. Recoveries averaged 93% at both levels of fortification. Coefficient method variation on both levels is
Makoto et al (1994) studied 10 multiresidue procedure for organophosphorus pesticides in the establishment of methods analytical gas chromatography on capillary column with flame photometric (FPD) and a detector mass spectrometry (GC-MS). chromatography gas phase with quantitative ODF was examined to determine the conditions multicolumn chromatography GC. gas chromatography GC-MS has been studied to select fragment ions suitable for the determination and identification.

Estimated GC-MS/LC-MS

Because the mass spectrometer is capable of achieving higher levels of molecular specificity compared to traditional GC detectors and can be programmed to Search hundreds of objects ions, GC / MS is a promising method for the regulators to explore residue monitoring pesticides in food per day (Cheng et al, 1994).

Cheng et al (1994) reported a multiresidue method using spectrometry mass gas chromatography / selected ion monitoring (GC / MS / SIM) for the determination of captan, chlorothalonil, dichlorovos, dimethoate, EPN, phorate, primiphos prothiophos-methyl residues in fruits and vegetables. The recoveries were between 46 and 108% at a dose of 0.5 mg / kg of each enrichment level of pesticides in apples, cabbage, cucumbers and grapes. The coefficients of variation are between 0.7 and 19%, with an average 7.5%. It is estimated that the detection limits of pesticides on crops were 0.1 to 0.05 mg / kg, except that the limit of detection of capture was more higher than in the culture of 0.5 mg / kg.

A method based on solid phase extraction cartridge and investment carbograph spectrometry phase liquid chromatography mass (LC / MS) with electrospray (ES) interface has been described by Corcia et al (1996) for trace Measurement of N-methylcarbamate insecticides in 10 different types of fruits and vegetables. carbamates added noon on plant material were extracted with methanol using a homogenizer followed by filtration, an aliquot of homogenate equivalent to 5 g of material plant has been well diluted with water and passed through January 1 Carbograpg an extraction thimble. Carbamates were eluted from 6 ml cartridge CH2Cl2/CH3OH (80:20 v / vegetables) mixture. The recovery of analytes was greater than 80%, whatever the type plant on which the parent analytes were added.

A method that uses solid phase extraction fully automated (SPE) purification samples and analysis in line liquid chromatography with UV and fluorescence detection in tandem for the determination of carbendazim and thiabendazole in different cultures has been reported by Hiemstra et al (1995).

In total, 199 pesticides have been determined by Fillion et al (1995) in fruits and vegetables by using acetonitrile as solvent extraction and cleaning of the column chromatography miniature charcoal celite Mass screening and gas selective ion monitoring mode. Carbamates were analyzed by liquid chromatography with post-column reaction and fluorescence detection. Recovery data were obtained by fortifying three matrices (pear, carrot and banana) from 0.1 to 0.5 ppm.

Blasco et al (2004) using a quantitative matrix solid phase dispersion and chemical liquid chromatography, mass spectrometry atmospheric ionization pressure (LC-APCI-MS) method for the simultaneous analysis of dithiocarbamates and their degradation products in crops. average recoveries ranging from 33 to 109% and relative standard deviation was between 4 and 21% with limits of quantification ranged from 0.25 to 2.5 mg / kg.

An analysis of waste Multiple determination of 101 pesticides, including organophosphates, organochlorine and nitrogen-containing pesticides in crops by chromatography gas phase mass selective detector gas was made by Chun et al (2003). The analysis is performed in the control mode selected ion. The samples were spiked with pesticides at 0.1 to 1.0 mg / kg. Recoveries of 90% of pesticides Wee between 70 and 110%, however, the recovery acephate and folpet were very poor, ie
An analysis of several residues broadband analysis of pesticides consists of extraction with ethyl acetate and a single column cartridge (consisting of two layers of water absorbent polymers (Top) graphitized carbon dioxide ()) the cleaning procedure in non-fatty vegetables and fruits has been developed by Oban et al (2001). In A recovery test, 110 pesticides were spiked and average recoveries were more than 95% of spinach and orange. Most pesticides were found in the range of 70-115% with a standard deviation usually
Simultaneous and consecutive methods of analysis Pesticide residues in food samples by acetonitrile extraction of many, followed by gel chromatography (GPC) and the mini-column cartridge cleaning then double-column GC equipped with ECD has been studied by Ueno et al (2004). Recoveries of 58 pesticides fortified spinach, tomatoes, apples and strawberries were very good (70-121%), except for acrinathrin, captan, captafol, and dichlofluanid etridiazole (
Simultaneous determination residues of 251 pesticides and degradation products of fruit and vegetable samples using gas chromatography with mass selective detection mode and selected ion monitoring liquid chromatography with post-column reaction and fluorescence detection of N-methyl carbamates after acetonitrile extraction and octadecyl (C18), cleaning cartridge solid phase extraction and cleaning one second, with a cartridge carbon with an amino propyl cartridge has been described by Fillion et al (2004). Limits of detection range between 0.02 and 1.0 mg / kg for most compounds. Over 80% of the compounds have a limit of detection _0.04 mg / kg.

Aguera et al (2002) by gas chromatography using a combination the positive chemical ionization (PCI) and electron impact (EI) ionisation modes and tandem mass spectrometry (GC-PCI/EI-MS-MS) as a test method for determining 55 organochlorine and organophosphorus and pyrethroids used in crop protection. Waste pesticide samples were extracted with a mixture of ethyl acetate and sodium sulfate, the final concentration of the sample after 1 mg / ml extract. No additional cleaning measures were necessary. Good sensitivity and selectivity of the method have been obtained with limits of detection ranging from 0.07 to 4.21 mg / kg in all cases, except for methamidophos, permethrin, cypermethrin and difenconazol] difenoconazole [. Average recoveries between 52 and 114% were obtained and showed a good linearity in the range studied (r_0.994).

A simple, rapid and sensitive multiresidue for the determination of ten organophosphorus pesticides Organochlorine extraction with ethyl acetate followed by an injection miniaturized high volume (10 mL) by GC-MS analysis in EI SIM (selective ion monitoring) was mode developed by Aguera et al (2004). The sensitivity and selectivity of the method are acceptable, with limits of detection (LOD) of less than 0.01 mg kg-1, with the exception of alpha and beta endosulfan (0.05 mg / kg). average recovery of 63-99% were obtained and showed good linearity in the range of 0.01 to 1.00 mg per kg 1.Repeatability and reproducibility studies gave relative standard deviations were less 20% in all cases. The method was applied to the analysis of 110 samples of vegetables, as part of the monitoring program of the Association Producers and exporters of fruits and vegetables in Almería.

A multi-residue method of pesticides that allows the quantitative analysis in the order of many vegetables and fruit samples by gas chromatography / mass spectrometry was reported by Ueno et al (2004). The sample was extracted with acetonitrile and the extract was cleaned by a step to be followed by redissolution in acetate ethyl salt. Coextractives be automatically removed by gel permeation chromatography with graphitized carbon column, followed by a tandem column silica-gel/PSA cartridge. Recoveries of 82 of the 89 pesticides fortified spinach, tomato, apple, strawberries were in the range of 70-120%, and were deviation values for 80 of the 89 pesticides
The analysis of the methanol extract, without additional cleaning steps are performed using tandem mass spectrometry-liquid chromatography electrospray ionization mode that combines positive and negative ions for the determination of a group of 16 multiclass pesticides most commonly used in crop protection. The extraction step was performed with a mixture ethyl acetate and sodium sulfate in the presence of 6.5 M NaOH. The recoveries were obtained on average between 70 and 110% in most cases with a accuracy
A new method of liquid chromatography mass spectrometry tandem for the routine analysis of pesticide residues of 31 multi-class and applies to approximately 50 samples of fruits and vegetables (green beans, cucumber, pepper, tomato, eggplant, watermelon, melon and zucchini) was developed by Garrido et al (2004). Extraction of pesticides with ethyl acetate was conducted. The average recoveries in cucumber obtained for each pesticide ranged between 74 and 105% at two different levels of enrichment (n = 10 each) that ranged between 9 and 250 ng g -1 (depending on product.) The uncertainty associated with the method of analysis was lower at 23% for all compounds tested. The calculated limits of detection and quantification are usually

Draft workplan

Standardization of methods of analysis Multiresidue pesticide for

Pesticides belonging to some standard analytical knowledge, the different classes. OC (HCH isomer (?,?,? Y?), DDT (OP-DDT, PP-DDT, op-DDD, pp-DDE), endosulfan ("," Y endosulfan sulfate) and dicofol), OP (Dimethoate, malathion, parathion-methyl , Chlorpyrifos, quinalphos Triazophos, Phosphamidon, dichlorvos and monocrotophos Metasystox) and synthetic pyrethroids (cypermethrin, deltamethrin, fenvalerate) in monitoring and decontamination studies were collected from various sources as follows:

SL No. Name Pesticide Source% purity

Organochlorines

1?-HCH 99.5 EPA

2?-HCH 99.5 EPA

3?-HCH 99.5 EPA

4?-HCH 99.5 EPA

EPA OP-DDT 99.7 5

99.7 6 PP-DDT EPA

EPA 7 OP-DDD 99.7

PP-DDE 99.7 8 EPA

9?-Endosulfan Excel 99.0

10 "" Excel 99.0 endosulfan

11 endosulfan sulfate 99.0 Excel

Bayer 12 96.0 dicofol

Organophosphates

Dimethoate 13 96.5 UPL

Malathion 14 97.3 UPL

Parathion-methyl 15 98.5 Bayer

Chlorpyrifos 16 99.7 Crop Protection Denocil Ltd.

Sandoz Ltd. 17 95.6 quinalphos

18 93.9 Bayer Phosphamidon

19 40.8 Triazophos Aventis Crop Science

Monocrotophos 20 77.0 UPL

Dichlorvos 21 -

22 Metasystox -

Synthetic pyrethroids CCSRI

Cypermethrin, 99.0 CCSRI

Deltamethrin

99.0 Fenvalerate

99.0 CCSRI

4.1.1 stock standard solution: standard solution of the mother of different pesticides must be prepared in distilled hexane / acetone and diluted appropriately to serve as a working model and verify the peaks chromatographic mindividual their ability to multi-residue analysis.

4.1.2 Preparation of standard mixed Solyte: from individual solutions standard, a standard mixed solution was prepared and sanitation mdevelopment method studies.

4.1.3 Extraction and cleanup

From the review of the literature three methods proposed by Kole et al (1998) Nakamura et al (1994) and Oban et al (2001) were chosen to perform the extraction and cleaning procedures that two liquid-liquid extraction column cartridge solid phase will be compared to develop a simple, rapid and cost to detect a wide range of pesticides.

4.1.4 Estimation of multi-residue pesticide

A gas chromatograph coupled an electron capture detector (ECD) and nitrogen-phosphorus detector (NPD) to be used for estimating residue pesticides. The operating conditions will also be considered as shown in the three methods chosen.

4.1.5 Standardization of Mathod:

This opens the selected method should be standardized by performing a recovery study with the standard mixed nailing in fruits and vegetables.

4.2 Monitoring of pesticide residues

4.2.1 sampling program:

TYPA sampled fruit (mango and banana) and vegetables (tomatoes, peppers, Caulioflower, col).

The sampling area: From 2 wholesale markets known as ... ... .. Bengal West.

The frequency and duration of sampling: Once per month for one year.

Sample volume: 1 kg each sample.

4.2.2 Control of pesticide residues: All pesticides listed in Table 2.

4.3 Study decontamination

Pesticides should be selected on the basis of their model a greater use of the SA BM] some pesticides are: CO (?-Endosulfan? Endosulfan sulfate endosulfan, dicofol OP: chlorpyrifos, quinalphos Dimethoate, Triazophos, malathion, methyl parathion, phosphamidon, monocrotophos, metasystix; synthetic pyrethroid: cypermethrin, deltamethrin and fenvalerate.

4.3.1 Decontamination procedures to be followed:

4.3.1.1 washed with water samples are collected, chopped into a tank containing water and the material is rubbed gently with water for about one minute and the water is decanted and rinsed in running water for 130 seconds. with a rotation of the gentle hand. washing was repeated two or three times.

4.3.1.2 washing with salt water cut samples immersed in a beaker containing 2 or 55% sodium chloride. After 10-15 minutes, the plant is rubbed gently by hand samplws in saline and salt water was decanted. Then the samples were was washed with water.

4.3.1.3 Boiling / Cooking: Wil unwashed samples being bitten and boiled in a beaker until the water evaporates completely covering the ContainR with or without lids. The samples were allowed to cool.

4.3.1.4 Combination previous methods such as soaking in water for 15 min., Rinse with water, cut into pieces and boiled in water

4.3.1.5 Wash in soapy water, rinse with water.

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