CN116298048A - Synchronous detection method for pesticide residues in Chinese chives - Google Patents
Synchronous detection method for pesticide residues in Chinese chives Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- high performance
- liquid chromatography
- performance liquid
- mass spectrometry
- synchronous detection
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000001514 detection method Methods 0.000 title claims abstract description 34
- 235000018645 Allium odorum Nutrition 0.000 title claims abstract description 29
- 235000005338 Allium tuberosum Nutrition 0.000 title claims abstract description 29
- 240000008654 Allium ramosum Species 0.000 title claims abstract description 24
- 239000000447 pesticide residue Substances 0.000 title claims abstract description 16
- 230000001360 synchronised effect Effects 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 12
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 claims abstract description 12
- OQKFGIANPCRSSK-UHFFFAOYSA-N azanium;methanol;acetate Chemical compound [NH4+].OC.CC([O-])=O OQKFGIANPCRSSK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000575 pesticide Substances 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000004949 mass spectrometry Methods 0.000 claims description 9
- XBJFCYDKBDVADW-UHFFFAOYSA-N acetonitrile;formic acid Chemical compound CC#N.OC=O XBJFCYDKBDVADW-UHFFFAOYSA-N 0.000 claims description 7
- 240000006108 Allium ampeloprasum Species 0.000 claims description 6
- 235000005254 Allium ampeloprasum Nutrition 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000005906 Imidacloprid Substances 0.000 claims description 4
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 claims description 4
- 229940056881 imidacloprid Drugs 0.000 claims description 4
- LCCNCVORNKJIRZ-UHFFFAOYSA-N parathion Chemical compound CCOP(=S)(OCC)OC1=CC=C([N+]([O-])=O)C=C1 LCCNCVORNKJIRZ-UHFFFAOYSA-N 0.000 claims description 4
- QNBTYORWCCMPQP-JXAWBTAJSA-N (Z)-dimethomorph Chemical compound C1=C(OC)C(OC)=CC=C1C(\C=1C=CC(Cl)=CC=1)=C/C(=O)N1CCOCC1 QNBTYORWCCMPQP-JXAWBTAJSA-N 0.000 claims description 3
- PXMNMQRDXWABCY-UHFFFAOYSA-N 1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol Chemical compound C1=NC=NN1CC(O)(C(C)(C)C)CCC1=CC=C(Cl)C=C1 PXMNMQRDXWABCY-UHFFFAOYSA-N 0.000 claims description 3
- HZJKXKUJVSEEFU-UHFFFAOYSA-N 2-(4-chlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)hexanenitrile Chemical compound C=1C=C(Cl)C=CC=1C(CCCC)(C#N)CN1C=NC=N1 HZJKXKUJVSEEFU-UHFFFAOYSA-N 0.000 claims description 3
- SOUGWDPPRBKJEX-UHFFFAOYSA-N 3,5-dichloro-N-(1-chloro-3-methyl-2-oxopentan-3-yl)-4-methylbenzamide Chemical compound ClCC(=O)C(C)(CC)NC(=O)C1=CC(Cl)=C(C)C(Cl)=C1 SOUGWDPPRBKJEX-UHFFFAOYSA-N 0.000 claims description 3
- RQDJADAKIFFEKQ-UHFFFAOYSA-N 4-(4-chlorophenyl)-2-phenyl-2-(1,2,4-triazol-1-ylmethyl)butanenitrile Chemical compound C1=CC(Cl)=CC=C1CCC(C=1C=CC=CC=1)(C#N)CN1N=CN=C1 RQDJADAKIFFEKQ-UHFFFAOYSA-N 0.000 claims description 3
- TWFZGCMQGLPBSX-UHFFFAOYSA-N Carbendazim Natural products C1=CC=C2NC(NC(=O)OC)=NC2=C1 TWFZGCMQGLPBSX-UHFFFAOYSA-N 0.000 claims description 3
- 239000005944 Chlorpyrifos Substances 0.000 claims description 3
- 239000005759 Diethofencarb Substances 0.000 claims description 3
- 239000005760 Difenoconazole Substances 0.000 claims description 3
- 239000005761 Dimethomorph Substances 0.000 claims description 3
- 239000005775 Fenbuconazole Substances 0.000 claims description 3
- 239000005807 Metalaxyl Substances 0.000 claims description 3
- 239000005811 Myclobutanil Substances 0.000 claims description 3
- 239000005820 Prochloraz Substances 0.000 claims description 3
- 239000005822 Propiconazole Substances 0.000 claims description 3
- 239000005869 Pyraclostrobin Substances 0.000 claims description 3
- 239000005828 Pyrimethanil Substances 0.000 claims description 3
- 239000005839 Tebuconazole Substances 0.000 claims description 3
- 239000005846 Triadimenol Substances 0.000 claims description 3
- 239000005857 Trifloxystrobin Substances 0.000 claims description 3
- 239000005863 Zoxamide Substances 0.000 claims description 3
- 239000006013 carbendazim Substances 0.000 claims description 3
- JNPZQRQPIHJYNM-UHFFFAOYSA-N carbendazim Chemical compound C1=C[CH]C2=NC(NC(=O)OC)=NC2=C1 JNPZQRQPIHJYNM-UHFFFAOYSA-N 0.000 claims description 3
- SBPBAQFWLVIOKP-UHFFFAOYSA-N chlorpyrifos Chemical compound CCOP(=S)(OCC)OC1=NC(Cl)=C(Cl)C=C1Cl SBPBAQFWLVIOKP-UHFFFAOYSA-N 0.000 claims description 3
- LNJNFVJKDJYTEU-UHFFFAOYSA-N diethofencarb Chemical compound CCOC1=CC=C(NC(=O)OC(C)C)C=C1OCC LNJNFVJKDJYTEU-UHFFFAOYSA-N 0.000 claims description 3
- BQYJATMQXGBDHF-UHFFFAOYSA-N difenoconazole Chemical compound O1C(C)COC1(C=1C(=CC(OC=2C=CC(Cl)=CC=2)=CC=1)Cl)CN1N=CN=C1 BQYJATMQXGBDHF-UHFFFAOYSA-N 0.000 claims description 3
- ZNOLGFHPUIJIMJ-UHFFFAOYSA-N fenitrothion Chemical compound COP(=S)(OC)OC1=CC=C([N+]([O-])=O)C(C)=C1 ZNOLGFHPUIJIMJ-UHFFFAOYSA-N 0.000 claims description 3
- FQKUGOMFVDPBIZ-UHFFFAOYSA-N flusilazole Chemical compound C=1C=C(F)C=CC=1[Si](C=1C=CC(F)=CC=1)(C)CN1C=NC=N1 FQKUGOMFVDPBIZ-UHFFFAOYSA-N 0.000 claims description 3
- ZQEIXNIJLIKNTD-UHFFFAOYSA-N methyl N-(2,6-dimethylphenyl)-N-(methoxyacetyl)alaninate Chemical compound COCC(=O)N(C(C)C(=O)OC)C1=C(C)C=CC=C1C ZQEIXNIJLIKNTD-UHFFFAOYSA-N 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 3
- TVLSRXXIMLFWEO-UHFFFAOYSA-N prochloraz Chemical compound C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl TVLSRXXIMLFWEO-UHFFFAOYSA-N 0.000 claims description 3
- QXJKBPAVAHBARF-BETUJISGSA-N procymidone Chemical compound O=C([C@]1(C)C[C@@]1(C1=O)C)N1C1=CC(Cl)=CC(Cl)=C1 QXJKBPAVAHBARF-BETUJISGSA-N 0.000 claims description 3
- STJLVHWMYQXCPB-UHFFFAOYSA-N propiconazole Chemical compound O1C(CCC)COC1(C=1C(=CC(Cl)=CC=1)Cl)CN1N=CN=C1 STJLVHWMYQXCPB-UHFFFAOYSA-N 0.000 claims description 3
- HZRSNVGNWUDEFX-UHFFFAOYSA-N pyraclostrobin Chemical compound COC(=O)N(OC)C1=CC=CC=C1COC1=NN(C=2C=CC(Cl)=CC=2)C=C1 HZRSNVGNWUDEFX-UHFFFAOYSA-N 0.000 claims description 3
- ZLIBICFPKPWGIZ-UHFFFAOYSA-N pyrimethanil Chemical compound CC1=CC(C)=NC(NC=2C=CC=CC=2)=N1 ZLIBICFPKPWGIZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004308 thiabendazole Substances 0.000 claims description 3
- WJCNZQLZVWNLKY-UHFFFAOYSA-N thiabendazole Chemical compound S1C=NC(C=2NC3=CC=CC=C3N=2)=C1 WJCNZQLZVWNLKY-UHFFFAOYSA-N 0.000 claims description 3
- 229960004546 thiabendazole Drugs 0.000 claims description 3
- 235000010296 thiabendazole Nutrition 0.000 claims description 3
- BAZVSMNPJJMILC-UHFFFAOYSA-N triadimenol Chemical compound C1=NC=NN1C(C(O)C(C)(C)C)OC1=CC=C(Cl)C=C1 BAZVSMNPJJMILC-UHFFFAOYSA-N 0.000 claims description 3
- ONCZDRURRATYFI-TVJDWZFNSA-N trifloxystrobin Chemical compound CO\N=C(\C(=O)OC)C1=CC=CC=C1CO\N=C(/C)C1=CC=CC(C(F)(F)F)=C1 ONCZDRURRATYFI-TVJDWZFNSA-N 0.000 claims description 3
- ZQEIXNIJLIKNTD-GFCCVEGCSA-N metalaxyl-M Chemical compound COCC(=O)N([C@H](C)C(=O)OC)C1=C(C)C=CC=C1C ZQEIXNIJLIKNTD-GFCCVEGCSA-N 0.000 claims description 2
- 239000002516 radical scavenger Substances 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 10
- 239000012071 phase Substances 0.000 description 9
- 201000011243 gastrointestinal stromal tumor Diseases 0.000 description 7
- 244000003377 Allium tuberosum Species 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012629 purifying agent Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 235000013311 vegetables Nutrition 0.000 description 3
- 241000238631 Hexapoda Species 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- NFGXHKASABOEEW-UHFFFAOYSA-N 1-methylethyl 11-methoxy-3,7,11-trimethyl-2,4-dodecadienoate Chemical compound COC(C)(C)CCCC(C)CC=CC(C)=CC(=O)OC(C)C NFGXHKASABOEEW-UHFFFAOYSA-N 0.000 description 1
- ZSBXGIUJOOQZMP-UHFFFAOYSA-N Isomatrine Natural products C1CCC2CN3C(=O)CCCC3C3C2N1CCC3 ZSBXGIUJOOQZMP-UHFFFAOYSA-N 0.000 description 1
- 241000234280 Liliaceae Species 0.000 description 1
- ZSBXGIUJOOQZMP-JLNYLFASSA-N Matrine Chemical compound C1CC[C@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-JLNYLFASSA-N 0.000 description 1
- RQBBFKINEJYDOB-UHFFFAOYSA-N acetic acid;acetonitrile Chemical compound CC#N.CC(O)=O RQBBFKINEJYDOB-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 229930014456 matrine Natural products 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229950003442 methoprene Drugs 0.000 description 1
- 229930002897 methoprene Natural products 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- WPALTCMYPARVNV-UHFFFAOYSA-N tolfenpyrad Chemical compound CCC1=NN(C)C(C(=O)NCC=2C=CC(OC=3C=CC(C)=CC=3)=CC=2)=C1Cl WPALTCMYPARVNV-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310492335.9A CN116298048A (en) | 2023-05-05 | 2023-05-05 | Synchronous detection method for pesticide residues in Chinese chives |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310492335.9A CN116298048A (en) | 2023-05-05 | 2023-05-05 | Synchronous detection method for pesticide residues in Chinese chives |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116298048A true CN116298048A (en) | 2023-06-23 |
Family
ID=86836253
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310492335.9A Pending CN116298048A (en) | 2023-05-05 | 2023-05-05 | Synchronous detection method for pesticide residues in Chinese chives |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116298048A (en) |
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 |
-
2023
- 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Acosta-Dacal et al. | Optimization and validation of a QuEChERS-based method for the simultaneous environmental monitoring of 218 pesticide residues in clay loam soil | |
| Lee et al. | Rapid and simultaneous analysis of 360 pesticides in brown rice, spinach, orange, and potato using microbore GC-MS/MS | |
| Carpinteiro et al. | Determination of fungicides in wine by mixed-mode solid phase extraction and liquid chromatography coupled to tandem mass spectrometry | |
| EP3593128A1 (en) | Polar pesticide determination using chromatography | |
| Cheng et al. | Simultaneous determination of fipronil and its major metabolites in corn and soil by ultra-performance liquid chromatography-tandem mass spectrometry | |
| CN107576741B (en) | Method for detecting organophosphorus pesticide multi-component residues in aquatic product by solid phase extraction-gas chromatography tandem mass spectrometry | |
| CN114127552B (en) | Improving recovery of organic compounds in liquid samples using pervaporation vacuum extraction, thermal desorption and GCMS analysis | |
| Paranthaman et al. | Determination of pesticide residues in banana by using high performance liquid chromatography and gas chromatography-mass spectrometry | |
| CN116298048A (en) | Synchronous detection method for pesticide residues in Chinese chives | |
| Zhang et al. | Disposable pipette extraction (DPX) coupled with liquid chromatography–tandem mass spectrometry for the simultaneous determination of pesticide residues in wine samples | |
| Argauer et al. | Determining propoxur and other carbamates in meat using HPLC fluorescence and gas chromatography/ion trap mass spectrometry after supercritical fluid extraction | |
| Pang et al. | High-throughput analytical techniques for multiresidue, multiclass determination of 653 pesticides and chemical pollutants in tea—part III: evaluation of the cleanup efficiency of an SPE cartridge newly developed for multiresidues in tea | |
| Li | Analytical methods for the analysis of volatile natural products | |
| Kimura et al. | Simple and rapid determination of 1‐deoxynojirimycin in mulberry leaves | |
| Hewavitharana et al. | Quantitative GC-MS analysis of Δ9-tetrahydrocannabinol in fiber hemp varieties | |
| CN104713974A (en) | Method for determining 55 kinds of pesticide residues in vegetable | |
| Castro et al. | Determination of chlormequat in fruit samples by liquid chromatography-electrospray-mass spectrometry/mass spectrometry | |
| Garau et al. | Residue-free wines: fate of some quinone outside inhibitor (QoI) fungicides in the winemaking process | |
| Hiemstra et al. | Determination of benzoylphenylurea insecticides in pome fruit and fruiting vegetables by liquid chromatography with diode array detection and residue data obtained in the Dutch national monitoring program | |
| Young et al. | Mixed-mode solid-phase extraction and cleanup procedures for the liquid chromatographic determination of thiabendazole and carbendazim in fruit juices | |
| Chagas et al. | Use of mass spectrometry for the determination of formaldehyde in samples potentially toxic to humans: a brief review | |
| CN105181870A (en) | Method for determining hymexazol residues in vegetables and fruits | |
| Rezk et al. | Selective determination of diazinon and chlorpyrifos in the presence of their degradation products: Application to environmental samples | |
| CN112255327A (en) | Method for detecting glufosinate content in dairy product | |
| Kang et al. | Analysis of total aflatoxins in spices and dried fruits |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |