CN1959406A - Method for detecting residue of Metalaxyl, badistan, thiophanate-methyl in vegetable - Google Patents

Abstract

A method for detecting residual of methylin and carbendazim as well as methosufate in vegetables includes steps of sampling, extracting, preparing standard curve and detecting; utilizing 236nm as detection wavelength for detecting out residuals of three said agricultural chemicals in vegetables in only one time of detection.

Description

Metalaxyl, carbendazim, thiophanate-methyl residual detection method in vegetables

Technical field:

The present invention relates to a kind of method that detects bactericide agricultural chemicals amount in the vegetables.

Background technology:

Generally once can only measure a kind of residual quantity of agricultural chemicals in the prior art to metalaxyl, carbendazim, thiophanate-methyl residual detection method in vegetables, three kinds of agricultural chemicals need carry out at least three times and detect, and job step complexity, detection sensitivity are also undesirable.

Summary of the invention:

The object of the present invention is to provide a kind of metalaxyl residual in the vegetables, carbendazim, thiophanate-methyl one-time detection can being come out, easy to detect, the high metalaxyl of accuracy, carbendazim, thiophanate-methyl residual detection method in vegetables.

Technical solution of the present invention is:

A kind of metalaxyl, carbendazim, thiophanate-methyl residual detection method in vegetables is characterized in that: comprise the following steps: successively

1. sampling: get and be no less than the 1000g vegetable sample, get edible part, wipe the attachment of sample surfaces gently, adopt the diagonal line split plot design, get the diagonal angle part, with its chopping, fully mixing is put into food processing equipment and is pulverized, and makes sample, puts into the packing containers for future use;

2. extract: accurately take by weighing 20g dish sample, add the 20ml acetonitrile, use filter paper filtering after the homogenized in refiner, filtrate collecting is equipped with in the 50ml tool plug graduated cylinder of 3g～5g sodium chloride, after the vibration, at room temperature leaves standstill 10 minutes, makes acetonitrile phase and water layering;

3. with nh 2 column with 5ml acetonitrile prewashing conditioning, when solvent liquid level arrives post adsorbed layer surface, suck acetonitrile phase solution immediately, collect eluent after discarding 2～3ml solution, to be measured;

4. production standard curve: the metalaxyl, carbendazim, the thiophanate-methyl that are respectively 0.05mg/l, 0.1mg/l, 0.5mg/l, 1.0mg/l, 5.0mg/l with dilution instrument compound concentration mix mark solution, treat with instrument state stable after, with series standard solution sample introduction, retention time is qualitative, with peak area and standard specimen concentration production standard curve, the eluent that 3. step is collected carries out sample detection then, and external standard method is quantitative; The instrument condition of said determination is:

High performance liquid chromatograph Agilent HPLC1100

Dilution instrument GILSON 402

Diode array detector DAD wavelength 236

Chromatographic column Agilent TC-C ₁₈Analytical 4.6 * 250mm

5-Micron

20 ℃ of column temperatures

Moving phase acetonitrile: water=52: 48 (v/v)

Flow velocity 1ml/min

Sample size 10 μ l.

Can calculate residual quantity according to following formula:

$X=\frac{\mathrm{CV}\×1000}{M\×1000}$

In the formula: X---persticide residue in the sample; Mg/kg

C---the concentration of detected sample liquid; Ng/ul

V---add the acetonitrile volume that extracts in the sample; Ml

M---sample quality; g

The present invention can come out metalaxyl residual in the vegetables, carbendazim, thiophanate-methyl one-time detection, and is easy to detect, the accuracy height.Select 236nm as detecting wavelength, metalaxyl, carbendazim, three kinds of agricultural chemicals of thiophanate-methyl are good at the absorption whole structure of ultraviolet region, and disturbing factor is few.

The invention will be further described below in conjunction with drawings and Examples.

Fig. 1 is the thiophanate-methyl canonical plotting.

Fig. 2 is the carbendazim canonical plotting.

Fig. 3 is the metalaxyl canonical plotting.

Fig. 4 is 0.5mg/l metalaxyl, carbendazim, thiophanate-methyl mark liquid collection of illustrative plates.

Fig. 5 is 1.0mg/l metalaxyl, carbendazim, thiophanate-methyl mark liquid collection of illustrative plates.

Fig. 6 is the blank collection of illustrative plates of embodiment of the invention vegetable sample.

Fig. 7 is the vegetable sample collection of illustrative plates that is added to 0.2mg/l metalaxyl, carbendazim, thiophanate-methyl.

Fig. 8 is the vegetable sample collection of illustrative plates that is added to 1.0mg/l metalaxyl, carbendazim, thiophanate-methyl.

Fig. 9 is the vegetable sample collection of illustrative plates that is added to 5.0mg/l metalaxyl, carbendazim, thiophanate-methyl.

In the accompanying drawing: Area: area; Amount: amount; Jiajiliujunling: thiophanate-methyl; Duojunling: carbendazim; Jiashuangling: metalaxyl;

Embodiment:

A kind of metalaxyl, carbendazim, thiophanate-methyl residual detection method in vegetables comprises the following steps: successively

1. sampling: get and be no less than the 1000g vegetable sample, get edible part, wipe the attachment of sample surfaces gently, adopt the diagonal line split plot design, get the diagonal angle part, with its chopping, fully mixing is put into food processing equipment and is pulverized, and makes sample, puts into the packing containers for future use;

2. extract: accurately take by weighing 20g dish sample, add the 20ml acetonitrile, in refiner (model: use filter paper filtering IKA-T25) after the homogenized, filtrate collecting is equipped with in the 50ml tool plug graduated cylinder of 3g～5g sodium chloride, behind the thermal agitation, at room temperature left standstill 10 minutes, make acetonitrile phase and water layering;

3. with nh 2 column (500mg; 6ml; Agilent is made) with 5ml acetonitrile prewashing conditioning, when solvent liquid level arrives post adsorbed layer surface, suck acetonitrile phase solution immediately, collect eluent after discarding 2～3ml solution, to be measured;

4. production standard curve: the metalaxyl, carbendazim, the thiophanate-methyl that are respectively 0.05mg/l, 0.1mg/l, 0.5mg/l, 1.0mg/l, 5.0mg/l with dilution instrument compound concentration mix mark solution, treat with instrument state stable after, with series standard solution sample introduction, retention time is qualitative, with peak area and standard specimen concentration production standard curve, the eluent that 3. step is collected carries out sample detection then, and external standard method is quantitative; The instrument condition of said determination is:

High performance liquid chromatograph Agilent HPLC 1100

Dilution instrument GILSON 402

Diode array detector DAD wavelength 236

Chromatographic column Agilent TC-C ₁₈Analytical 4.6 * 250mm

5-Micron

20 ℃ of column temperatures

Moving phase acetonitrile: water=52: 48 (v/v)

Flow velocity 1ml/min

Sample size 10 μ l.

Can calculate residual quantity according to following formula:

$X=\frac{\mathrm{CV}\×1000}{M\×1000}$

In the formula: X---persticide residue in the sample; Mg/kg

C---the concentration of detected sample liquid; Ng/ul

V---add the acetonitrile volume that extracts in the sample; Ml

M---sample quality; G.

Be used in the reliability of the method validation the inventive method that adds 0.2～5.0mg/l metalaxyl, carbendazim, thiophanate-methyl in the vegetables blank sample, the result shows:

Add metalaxyl 0.2～5.0mg/kg in the recovery vegetables, the recovery is 78.52%～98.05%.Relative standard deviation (RSD) 1.32%～10.54%.Add carbendazim 0.2～5.0mg/kg, the recovery is 86.97%～112.74%.Relative standard deviation 1.01%～8.60%.Add thiophanate-methyl 0.2～5.0mg/kg, the recovery is 93.90%～111.14%.Relative standard deviation 3.01%～8.05%.Experimental result sees following table for details:

Pesticide name	Add concentration (mg/l)	Multiplicity	Measured concentration (mg/l)	The recovery (%)	RSD(％)
						Metalaxyl	0.2	1	0.1772	88.60	5.08
2	0.1887	94.35
			3	0.1961	98.05
1.0	1	0.8522						85.22	1.32
			2	0.8330	83.30
	3	0.8351					83.31
			5.0	1	4.8188			96.38		10.54
2	4.2173	84.35
				3	3.9260		78.52
Carbendazim	0.2	1						0.1970	98.50		1.01
			2	0.1993	99.65
		3				0.2010	100.50
			1.0	1	1.1102			111.02	1.76

		2	1.0884	108.84
						3	1.1274	112.74
		5.0	1	4.9900					99.80	8.60
	2				5.1241	102.48
			3	4.3485			86.97
	Thiophanate-methyl				0.2	1		0.1878	93.90		8.05
2		0.2112	105.60
				3		0.2199	109.95
1.0		1	1.0243					102.43	4.10
				2	1.1114	111.14
		3	1.0613				106.13
				5.0	1	5.1065		102.13		3.01
2		5.2176	104.35
					3	5.4170	108.34

This shows: the superiority one of this method is easy, the easy row of method; The 2nd, detection time is short, and three kinds of agricultural chemicals are measured in a pre-treatment and upper machine examination; The 3rd, it is few to consume chemical examination amount, and kind is also few.

Claims (1)

1, a kind of metalaxyl, carbendazim, thiophanate-methyl residual detection method in vegetables is characterized in that: comprise the following steps: successively

1. sampling: get and be no less than the 1000g vegetable sample, get edible part, wipe the attachment of sample surfaces gently, adopt the diagonal line split plot design, get the diagonal angle part, with its chopping, fully mixing is put into food processing equipment and is pulverized, and makes sample, puts into the packing containers for future use;

2. extract: accurately take by weighing 20g dish sample, add the 20ml acetonitrile, use filter paper filtering after the homogenized in refiner, filtrate collecting is equipped with in the 50ml tool plug graduated cylinder of 3g～5g sodium chloride, after the vibration, at room temperature leaves standstill 10 minutes, makes acetonitrile phase and water layering;

3. with nh 2 column with 5ml acetonitrile prewashing conditioning, when solvent liquid level arrives post adsorbed layer surface, suck acetonitrile phase solution immediately, collect eluent after discarding 2～3ml solution, to be measured;

4. production standard curve: the metalaxyl, carbendazim, the thiophanate-methyl that are respectively 0.05mg/l, 0.1mg/l, 0.5mg/l, 1.0mg/l, 5.0mg/l with dilution instrument compound concentration mix mark solution, treat with instrument state stable after, with series standard solution sample introduction, retention time is qualitative, with peak area and standard specimen concentration production standard curve, the eluent that 3. step is collected carries out sample detection then, and external standard method is quantitative; The instrument condition of said determination is:

High performance liquid chromatograph Agilent HPLC1100

Dilution instrument GILSON 402

Diode array detector DAD wavelength 236

Chromatographic column Agilent TC-C ₁₈Analytical 4.6 * 250mm

5-Micron

20 ℃ of column temperatures

Moving phase acetonitrile: water=52: 48 (v/v)

Flow velocity 1ml/min

Sample size 10 μ l.

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