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LC-MS/MS Determination Method for Simultaneous Detection of 7 Molluscicides in Vegetables and Fruits

A molluscicide, LC-MS technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of high cost, cumbersome and time-consuming pretreatment methods, single detection type, etc., and achieve the effect of saving time and cost.

Inactive Publication Date: 2015-10-28
JINAN CUSTOMS TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are domestic reports on the use of gas chromatography (GC-ECD) to detect insecticidal rings; reports on the use of LC-MS / MS to detect methocarb, which are aimed at aquatic products with high protein substrates such as puffer fish, eel and prawns; The report on the detection of metaldehyde by LC-MS / MS method is only for the vegetable matrix, and the pretreatment method is cumbersome, time-consuming and costly; "Detection and digestion dynamics of metaldehyde residues in tobacco and soil" The assay method for detecting metaldehyde in tobacco and soil is disclosed, but the detection types of the above method are relatively single, only involving one or two molluscicides, or the pretreatment method needs to be further improved; the author once established LC - MS / MS method for detection of insecticidal cyclocyclone, metaldehyde, and methiocarb, the detection target of this method only involves three molluscicides, and the pretreatment method needs to be further improved

Method used

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  • LC-MS/MS Determination Method for Simultaneous Detection of 7 Molluscicides in Vegetables and Fruits
  • LC-MS/MS Determination Method for Simultaneous Detection of 7 Molluscicides in Vegetables and Fruits
  • LC-MS/MS Determination Method for Simultaneous Detection of 7 Molluscicides in Vegetables and Fruits

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Determination of 7 molluscicides in Chinese cabbage samples.

[0085] 3 Sample extraction and purification

[0086] 3.1 Extraction

[0087] Weigh 10.00g (accurate to 0.01g) of blank cabbage samples and place them in 50mL centrifuge tubes, add three different concentrations of metaldehyde (10μg / kg, 20μg / kg, 50μg / kg) in the centrifuge tubes, Standard solutions of methiocarb, dimezocarb, sodium pentachlorophenate, snailicide, spirulina, and nicotinamide, set 6 parallels for each concentration level, accurately add 20mL of acetonitrile, and mix in the homogenizer at 10000r / min Homogenize for 1min, then add 3.0g sodium chloride to the centrifuge tube, homogenize for 1min again, place the centrifuge tube in a centrifuge, centrifuge at 3000r / min for 5min, draw 10mL of the supernatant into a 10mL centrifuge tube, place at 40 °C blown to dryness with nitrogen in a water bath. Accurately add 2.0 mL of acetonitrile to dissolve the residue and vortex for 2 min to be purified.

...

Embodiment 2

[0102] Determination of 7 molluscicides in strawberry samples.

[0103] 3 Sample extraction and purification

[0104] 3.1 Extraction

[0105] Weigh 10.00g (accurate to 0.01g) of blank strawberry samples and place them in 50mL centrifuge tubes, add metaldehyde with three different concentrations (10μg / kg, 20μg / kg, 50μg / kg) in the centrifuge tubes, Standard solutions of methiocarb, dimezocarb, sodium pentachlorophenate, snailicide, spirulina, and nicotinamide, set 6 parallels for each concentration level, accurately add 20mL of acetonitrile, and mix in the homogenizer at 10000r / min Homogenize for 1min, then add 3.5g sodium chloride to the centrifuge tube, homogenize for 1min again, place the centrifuge tube in a centrifuge, centrifuge at 3000r / min for 5min, draw 10mL of the supernatant into a 10mL centrifuge tube, place at 40 °C blown to dryness with nitrogen in a water bath. Accurately add 2.0 mL of acetonitrile to dissolve the residue and vortex for 2 min to be purified.

...

Embodiment 3

[0114] Determination of 7 molluscicides in spinach samples.

[0115] 3 Sample extraction and purification

[0116] 3.1 Extraction

[0117] Weigh 10.00g (accurate to 0.01g) blank spinach samples and place them in 50mL centrifuge tubes, add metaldehyde with three different concentrations (10μg / kg, 20μg / kg, 50μg / kg) in the centrifuge tubes, Standard solutions of methiocarb, dimezocarb, sodium pentachlorophenate, snailicide, spirulina, and nicotinamide, set 6 parallels for each concentration level, accurately add 20mL of acetonitrile, and mix in the homogenizer at 10000r / min Homogenize for 1min, then add 3.0g sodium chloride to the centrifuge tube, homogenize for 1min again, place the centrifuge tube in a centrifuge, centrifuge at 3000r / min for 5min, draw 10mL of the supernatant into a 10mL centrifuge tube, place at 40 °C blown to dryness with nitrogen in a water bath. Accurately add 2.0 mL of acetonitrile to dissolve the residue and vortex for 2 min to be purified.

[0118] 3...

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Abstract

The invention discloses an LC-MS / MS (liquid chromatography-mass spectrometry / mass spectrometry) measurement method for simultaneously detecting seven molluscicides in vegetables and fruits, and belongs to the technical field of analysis and detection. The seven molluscicides comprise niclosamide, thiocyclam, trifenmorph, nicotinanilide, sodium pentachlorophenate, mercaptodimethur and metaldehyde. According to the measurement method, acetonitrile is used for salting out and extraction, and PSA (polysialic acid) powder and C18 powder are used for purification; liquid chromatography-tandem mass spectrometry is used for simultaneously and quantitatively measuring the seven molluscicides in the vegetables and the fruits. The method is easy to operate, good in purification effect, high in sensitivity and high in repetitiveness and can be widely applied to residue detection on the seven molluscicides inclucing niclosamide, thiocyclam, trifenmorph, nicotinanilide, sodium pentachlorophenate, mercaptodimethur and metaldehyde in the vegetables and the fruits.

Description

technical field [0001] The invention relates to a method for simultaneously detecting multiple pesticide residues in fruits and vegetables, in particular to an LC-MS / MS method capable of simultaneously quantitatively determining seven molluscicides in vegetables and fruits. Background technique [0002] Pesticides used to control harmful molluscs such as snails, snails, and snails are called molluscicides. Since inorganic molluscicides such as copper sulfate and calcium arsenate have been discontinued, organic molluscicides are currently the main means of chemical control of molluscs. Organic molluscicides are divided into the following categories according to their chemical structures: ①Phenols: such as sodium pentachlorophenate and spirulina; ②Morpholines: such as snail killers; ③Organotins; Insecticidal ring (Cetrol); ⑤Others: such as metaldehyde, methoxacarb, nicotinamide. Among them, sodium pentachlorophenate and snails have been banned due to their extreme toxicity a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 郑新华何桂华韩焕美王乐张爱霞陈晞
Owner JINAN CUSTOMS TECH CENT