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Pretreatment and quantitative analysis method for rapid determination of pesticide residue in tea

A technology for rapid determination of pesticide residues, applied in the direction of measuring devices, analysis materials, material separation, etc., can solve the problems of long time-consuming and cumbersome detection methods, achieve good pigment removal, improve separation efficiency, and have wide application prospects

Active Publication Date: 2016-11-16
厦门鹭珈聚芯生物科技有限公司
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Problems solved by technology

At present, a variety of pretreatment methods for tea samples have been reported in the literature, such as gel permeation chromatography (GPC), solid-phase extraction (SPE), dispersive solid-phase extraction (DSPE), matrix solid-phase dispersive extraction (MSPD), solid-phase phase microextraction (SPME), etc. However, these methods are usually cumbersome, making the detection method too time-consuming

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  • Pretreatment and quantitative analysis method for rapid determination of pesticide residue in tea
  • Pretreatment and quantitative analysis method for rapid determination of pesticide residue in tea
  • Pretreatment and quantitative analysis method for rapid determination of pesticide residue in tea

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Embodiment 1

[0037] A pretreatment method for rapid determination of pesticide residues in tea,

[0038] 1) Extraction steps: Weigh 4.0g of homogenized tea samples into a 50mL centrifuge tube, add 10mL of pure water to soak for 30min, then add 20mL of acetonitrile, vortex for 1min; then add 4.0g of NaOAc and vortex for 1min, then Min speed centrifugation 5min, acetonitrile and water phase separation, the gained supernatant acetonitrile layer is the tea extract (such as Figure 1a shown);

[0039] 2) purification step: get 1mL tea extract in embodiment 1, add the magnesium sulfate (MgSO 4 ), vortexed for 1 min and then centrifuged, the supernatant collected was the tea purification solution ( Figure 1b ), which can be used as a test solution for rapid determination of pesticide residues in tea.

[0040] Compared with the traditional QuEChERS extraction method, comparative examples 1-3 are as follows:

Embodiment 2

[0051] A pretreatment method for rapid determination of pesticide residues in tea, the purification steps are as follows:

[0052] Get the 1mL tealeaves extract in embodiment 1, add the magnesium sulfate (MgSO 4 ), vortexed for 1 min and then centrifuged, the supernatant collected was the tea purification solution ( figure 2 ), which can be used as a test solution for rapid determination of pesticide residues in tea.

[0053] Compared with the traditional QuEChERS purification method, the comparative examples 4-5 are as follows:

Embodiment 3

[0062] At present, there are many types of pesticides used in the tea planting process. The present invention establishes a general-purpose detection method for rapid determination of pesticide residues in tea leaves. In this example, 69 commonly used pesticides (including organophosphorus, organochlorine, organic nitrogen, pyrethroids, phenylpyrazoles, etc.) for the investigation of this method. In order to obtain higher selectivity and sensitivity, this embodiment uses the standard solution of pesticides to optimize the precursor ions, product ions, and collision energy of pesticides in the GC-MS / MS analysis of this detection method. Two ion pairs were optimized for qualitative and quantitative analysis respectively, and the optimized results are shown in Table 3.

[0063] Table 3. Retention time, qualitative and quantitative transitions and collision voltage of 69 pesticides

[0064]

[0065]

[0066]

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Abstract

The invention discloses a pretreatment and quantitative analysis method for rapid determination of pesticide residue in tea. The method comprises the following steps: 1) extraction: soaking the tea in water, adding acetonitrile for extraction of pesticide residues, then adding sodium acetate for salting out, so as to separate an organic phase and a water phase and obtain an acetonitrile layer of a tea extract; 2) purification: step 1) adding activated carbon, N-Propylethylenediamine and magnesium sulfate in the tea extract for purification, so as to obtain a supernatant namely a liquid to be tested in the fast determination of pesticide residues in tea; and 3) using a standard curve method to conduct quantitative analysis by gas chromatography-tandem mass spectrometry. In the pretreatment process, the extract contains considerably reduced tea matrix; the purifying effect is good, and the recovery rate of pesticide is basically not affected, so as to greatly improve the pretreatment effect; and the gas chromatography-tandem mass spectrometry is combined for separation detection of the pesticide. The method greatly improves the separation efficiency of pesticide, reaches high detection sensitivity and accuracy and good reproducibility.

Description

technical field [0001] The invention belongs to the technical field of rapid analysis and detection, in particular to a pretreatment method and a quantitative analysis method for rapid determination of pesticide residues in tea. Background technique [0002] Tea is an important agricultural product of our country and also a traditional export commodity of our country. Because it has a unique aroma and contains many substances beneficial to the human body, it has become one of the most popular drinks in the world. However, in the process of tea plantation, there are many diseases and insect pests. In order to reduce the impact of pests and insects on the yield and quality of tea, various pesticides are inevitably used in the production process. These pesticides may eventually remain in the tea and bring harm to human health serious threat. Many countries and related agencies have stipulated the maximum residue levels (MRLs) of various pesticides in tea, so as to ensure the h...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/02
CPCG01N30/02G01N30/06G01N2030/025G01N2030/065
Inventor 彭西甜张惠贤鲁维夏虹胡西洲王小飞彭立军
Owner 厦门鹭珈聚芯生物科技有限公司
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