CN116298048A - Synchronous detection method for pesticide residues in Chinese chives - Google Patents
Synchronous detection method for pesticide residues in Chinese chives Download PDFInfo
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- CN116298048A CN116298048A CN202310492335.9A CN202310492335A CN116298048A CN 116298048 A CN116298048 A CN 116298048A CN 202310492335 A CN202310492335 A CN 202310492335A CN 116298048 A CN116298048 A CN 116298048A
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Abstract
The invention relates to the technical field of pesticide detection. The invention provides a synchronous detection method for pesticide residues in Chinese chives, which comprises the following steps: detecting the Chinese chives sample by high performance liquid chromatography-tandem mass spectrometry; in the high performance liquid chromatography process, 0.05-0.15% formic acid-4-6 mmol/L ammonium acetate-methanol is adopted as a mobile phase. The detection method disclosed by the invention adopts synchronous detection, can synchronously detect various common pesticide residues according to the needs, and has the advantages of high sensitivity, short detection time and accurate and reliable results.
Description
Technical Field
The invention relates to the technical field of pesticide detection, in particular to a synchronous detection method for pesticide residues in Chinese chives.
Background
The Chinese chives belong to perennial root vegetables of the lily family, have strong adaptability, are cold-resistant and heat-resistant, are widely planted, and can be produced throughout the year. The leaves, the flower and the flowers of the Chinese chives are all eaten as vegetables; seeds can be used as medicine, and has effects of invigorating kidney, invigorating stomach, refreshing, and suppressing sweating and astringing.
However, during the stage of planting, the Chinese chives belong to vegetables which are particularly easy to grow, are most easily damaged by soil insects such as Chinese chive maggots, grubs, cricket and the like in the growth process of the Chinese chives, and particularly, the insect which specially bites the soil stems, namely Chinese chive maggots, is fatal to the Chinese chives. The Chinese chive maggots often grow at the roots of Chinese chives, the pesticide sprayed is ineffective to the Chinese chive maggots, and the disinsection effect can be achieved only by applying the pesticide underground in a root irrigation mode and applying the pesticide to the roots of the Chinese chives and repeatedly irrigating the roots. This results in the possibility of illegal use of methoprene (3911), phoaphos (Su Hua 203) and parathion (1606) in addition to the allowed pesticides such as matrine aqua and imidacloprid during the planting process of leeks.
With the improvement of living standard, food safety is more and more important for people, and food detection needs are more and more important. Therefore, it is important to provide a method for detecting a plurality of kinds of objects with high detection accuracy.
Disclosure of Invention
The invention aims to provide a synchronous detection method for pesticide residues in Chinese chives, which can synchronously detect various common pesticides and improve detection efficiency and detection accuracy.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a synchronous detection method for pesticide residues in Chinese chives, which comprises the following steps: detecting the Chinese chives sample by high performance liquid chromatography-tandem mass spectrometry;
in the high performance liquid chromatography process, 0.05-0.15% formic acid-4-6 mmol/L ammonium acetate-methanol is adopted as a mobile phase.
Preferably, a Shi-pack GIST C18 column is used in the high performance liquid chromatography.
Preferably, the ionization mode in the mass spectrometry is ESI + 。
Preferably, the flow rate of nitrogen in the mass spectrometry is 12-25L/min, and the CDL temperature is 30-60 ℃.
Preferably, the high performance liquid chromatography-tandem mass spectrometry detection further comprises a pretreatment method of the leek sample; and during pretreatment, a full-automatic QuEChERS instrument is adopted for treatment.
Preferably, 80-120 mg C18+180-220 mg PSA+450-550 mg MgSO is used in the pretreatment 4 As a scavenger.
Preferably, 4-6% formic acid-acetonitrile solution is used as the extractant in the pretreatment.
Preferably, the types of the pesticides include: carbendazim, thiabendazole, diethofencarb, triadimenol, pyrimethanil, metalaxyl, mefenoxam, myclobutanil, tebuconazole, zoxamide, procymidone, flusilazole, dimethomorph, fenbuconazole, propiconazole, prochloraz, trifloxystrobin, difenoconazole, pyraclostrobin, tolfenpyr-methyl, fenitrothion, parathion, imidacloprid, chlorpyrifos.
The invention provides a synchronous detection method for pesticide residues in Chinese chives, which comprises the following steps: detecting the Chinese chives sample by high performance liquid chromatography-tandem mass spectrometry; in the high performance liquid chromatography process, 0.05-0.15% formic acid-4-6 mmol/L ammonium acetate-methanol is adopted as a mobile phase. The detection method disclosed by the invention adopts synchronous detection, can synchronously detect various common pesticide residues according to the needs, and has the advantages of high sensitivity, short detection time and accurate and reliable results.
Drawings
FIG. 1 shows the separation effect of a Shi-pack GIST C18 column;
FIG. 2 shows the separation effect of the phenomenomex bisphenyl column.
Detailed Description
The invention provides a synchronous detection method for pesticide residues in Chinese chives, which can synchronously detect various common pesticides and improve detection efficiency and detection accuracy.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a synchronous detection method for pesticide residues in Chinese chives, which comprises the following steps: detecting the Chinese chives sample by high performance liquid chromatography-tandem mass spectrometry;
in the high performance liquid chromatography, 0.05-0.15% formic acid-4-6 mmol/L ammonium acetate-methanol is preferably used as a mobile phase, and 0.1% formic acid-5 mmol/L ammonium acetate-methanol is more preferably used as a mobile phase.
In the present invention, the high performance liquid chromatography preferably uses a Shi-pack GIST C18 column.
In the present invention, the ionization mode in the mass spectrometry is preferably ESI + 。
In the present invention, the nitrogen flow rate during the mass spectrometry is preferably 12 to 25L/min, more preferably 15 to 20L/min, and the CDL temperature is preferably 30 to 60℃and more preferably 40 to 50 ℃.
In the invention, the detection by the high performance liquid chromatography-tandem mass spectrometry preferably further comprises a pretreatment method of a Chinese chive sample; the pretreatment is preferably performed by a fully automatic QuEChERS instrument.
In the present invention, 100mg C18+200mg PSA+500mg MgSO is preferably used for the pretreatment 4 The purifying agent is more preferably used.
In the present invention, a 4 to 6% formic acid-acetonitrile solution is preferably used as the extractant in the pretreatment, and a 5% formic acid-acetonitrile solution is more preferably used.
In the present invention, the types of the agricultural chemical preferably include: carbendazim, thiabendazole, diethofencarb, triadimenol, pyrimethanil, metalaxyl, myclobutanil, tebuconazole, zoxamide, procymidone, flusilazole, dimethomorph, fenbuconazole, propiconazole, prochloraz, trifloxystrobin, difenoconazole, pyraclostrobin, tolfenpyrad, fenitrothion, parathion, imidacloprid, and chlorpyrifos.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Using 80mg C18+220mg PSA+450mg MgSO 4 As a purifying agent, a 6% formic acid-acetonitrile solution is used as an extracting agent, and a full-automatic QuEChERS instrument is used for carrying out pretreatment on the leek sample;
detecting the pretreated sample by high performance liquid chromatography-tandem mass spectrometry;
in the high performance liquid chromatography process, 0.15 percent formic acid-4 mmol/L ammonium acetate-methanol is adopted as a mobile phase, and the high performance Shi-pack GIST C18 chromatographic column is utilized for carrying out;
ionization mode in mass spectrometry is ESI + The nitrogen flow rate was 25L/min and the CDL temperature was 30 ℃.
Example 2
Using 120mg C18+180mg PSA+550mg MgSO 4 As a purifying agent, 4% formic acid-acetonitrile solution is used as an extracting agent, and a full-automatic QuEChERS instrument is used for carrying out pretreatment on the leek sample;
detecting the pretreated sample by high performance liquid chromatography-tandem mass spectrometry;
in the high performance liquid chromatography process, 0.05 percent formic acid-6 mmol/L ammonium acetate-methanol is adopted as a mobile phase, and the high performance Shi-pack GIST C18 chromatographic column is utilized for carrying out;
ionization mode in mass spectrometry is ESI +， The nitrogen flow rate was 12L/min and the CDL temperature was 60 ℃.
Example 3
Using 100mg C18+200mg PSA+500mg MgSO 4 As a purifying agent, a 5% formic acid-acetonitrile solution is used as an extracting agent, and a full-automatic QuEChERS instrument is used for carrying out pretreatment on the leek sample;
detecting the pretreated sample by high performance liquid chromatography-tandem mass spectrometry;
in the high performance liquid chromatography process, 0.1 percent formic acid-5 mmol/L ammonium acetate-methanol is adopted as a mobile phase, and the high performance Shi-pack GIST C18 chromatographic column is utilized for carrying out;
ionization mode in mass spectrometry is ESI + The nitrogen flow rate was 20L/min and the CDL temperature was 45 ℃.
Test examples
Treating folium Allii tuberosi with QuEChERS method, extracting with 5% acetic acid-acetonitrile (1:99, V/V) solution, dispersing solid phase extraction adsorbent (100mg C18+200mg PSA+500mg MgSO) 4 ) Purifying, converting methanol solvent to constant volume, filtering with 0.22 μm filter membrane, separating with Shi-pack GIST C18 chromatographic column, taking 0.1% formic acid-5 mmol/L ammonium acetate-methanol as mobile phase, and qualitatively analyzing by retention time matching and accurate mass numbers of parent ion and main fragment ion, and quantifying by matrix standard solution external standard method. Under the optimized condition, the retention time of 24 pesticide residues is between 4.4 and 13.4 min. When the mass concentration range is 0.005 mug/mL-0.05 mug/mL, the linear relation of various pesticide residues is good, the correlation coefficient (r) is not less than 0.9990, the detection limit (S/N=3) of the method is 0.03 mug/kg-0.92 mug/kg, the quantitative limit is 0.50 mug/kg-2.10 mug/kg, the standard average recovery rate is 85% -110% on 3 concentration levels, and the relative standard deviation (n=6) is 2.8% -7.5%.
As can be seen from the above embodiments, the present invention provides a method for synchronously detecting pesticide residues in Chinese chives, which comprises the following steps: detecting the Chinese chives sample by high performance liquid chromatography-tandem mass spectrometry; in the high performance liquid chromatography process, 0.05-0.15% formic acid-4-6 mmol/L ammonium acetate-methanol is adopted as a mobile phase. The detection method disclosed by the invention adopts synchronous detection, can synchronously detect various common pesticide residues according to the needs, and has the advantages of high sensitivity, short detection time and accurate and reliable results.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. A synchronous detection method of pesticide residues in Chinese chives is characterized by comprising the following steps: detecting the Chinese chives sample by high performance liquid chromatography-tandem mass spectrometry;
in the high performance liquid chromatography process, 0.05-0.15% formic acid-4-6 mmol/L ammonium acetate-methanol is adopted as a mobile phase.
2. The synchronous detection method according to claim 1, wherein the high performance liquid chromatography process employs a Shi-packGISTC18 column.
3. The method according to claim 2, wherein the ionization mode in the mass spectrometry is ESI + 。
4. The method according to claim 3, wherein the nitrogen flow rate in the mass spectrometry is 12-25L/min and the CDL temperature is 30-60 ℃.
5. The method according to any one of claims 1 to 4, wherein the high performance liquid chromatography-tandem mass spectrometry detection further comprises a pretreatment method of leek samples; and during pretreatment, a full-automatic QuEChERS instrument is adopted for treatment.
6. The method for simultaneous detection according to claim 5, wherein 80-120 mgC18+180-220 mgPSA+450-550 mgMgSO is used in the pretreatment 4 As a scavenger.
7. The method according to claim 6, wherein the pretreatment is performed using a 4-6% formic acid-acetonitrile solution as the extractant.
8. The synchronous detection method according to claim 7, wherein the kind of the pesticide includes: carbendazim, thiabendazole, diethofencarb, triadimenol, pyrimethanil, metalaxyl, mefenoxam, myclobutanil, tebuconazole, zoxamide, procymidone, flusilazole, dimethomorph, fenbuconazole, propiconazole, prochloraz, trifloxystrobin, difenoconazole, pyraclostrobin, tolfenpyr-methyl, fenitrothion, parathion, imidacloprid, chlorpyrifos.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117809070A (en) * | 2024-03-01 | 2024-04-02 | 唐山市食品药品综合检验检测中心(唐山市农产品质量安全检验检测中心、唐山市检验检测研究院) | Spectral data intelligent processing method for detecting pesticide residues in vegetables |
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- 2023-05-05 CN CN202310492335.9A patent/CN116298048A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117809070A (en) * | 2024-03-01 | 2024-04-02 | 唐山市食品药品综合检验检测中心(唐山市农产品质量安全检验检测中心、唐山市检验检测研究院) | Spectral data intelligent processing method for detecting pesticide residues in vegetables |
| CN117809070B (en) * | 2024-03-01 | 2024-05-14 | 唐山市食品药品综合检验检测中心(唐山市农产品质量安全检验检测中心、唐山市检验检测研究院) | Spectral data intelligent processing method for detecting pesticide residues in vegetables |
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