CN108680688A - The assay method of BAC and DDAC in a kind of soil and plant-derived product - Google Patents
The assay method of BAC and DDAC in a kind of soil and plant-derived product Download PDFInfo
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- CN108680688A CN108680688A CN201810432201.7A CN201810432201A CN108680688A CN 108680688 A CN108680688 A CN 108680688A CN 201810432201 A CN201810432201 A CN 201810432201A CN 108680688 A CN108680688 A CN 108680688A
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Abstract
The invention discloses the assay methods of BAC and DDAC in soil and plant-derived product a kind of, as follows using liquid chromatography tandem mass spectrometry, including extraction, purification, three step of examination with computer, specific following steps：1) it extracts, weighs sample in 50mL plastic centrifuge tubes, 5 20mL water are added, 5 20mL methanol, vortex mixing are added in vortex mixing, and saturated nacl aqueous solution is added in ultrasound, and centrifugation takes supernatant, is repeated once, and merges supernatant, to be clean；2) it purifies, pipettes above-mentioned supernatant, cross SPE purification pipes, purify in pipe and 50 500mgGCB powder, 50 500mgC18 powder and 50 500mgPSA powder are added, be fully vortexed mixing, and centrifugation obtains second of supernatant；3) examination with computer takes second of supernatant, nitrogen to be blown to dry, addition 1mL water redissolution, excessively film, for liquid chromatography tandem mass spectrograph measurement.The present invention disposably can effectively detect 9 kinds of different compound residuals simultaneously, and detection sensitivity is high, and detection limit is low.
Description
Technical field
The present invention relates to a kind of assay method, more particularly to the survey of BAC and DDAC in a kind of soil and plant-derived product
Determine method.
Background technology
Currently, existing national standard only has GB/T30931-2014 to being utilized in efficient liquid chromatography cosmetics
The measurement of benzalkonium chloride content, and BAC and DDAC has 9 kinds of different chemical combination of two major classes in soil and in plant-derived product
Object remains, and there is no the assay method to BAC and DDAC in soil and plant-derived product, plant-derived products in existing standard
Generally include fruit and vegetables etc..
Invention content
To solve the problems, such as above-mentioned background technology, the purpose of the present invention is to provide a kind of soil and plant-derived
The assay method of BAC and DDAC in product is remained, inspection with reaching while disposably can effectively detect 9 kinds of different compounds
Survey high sensitivity, the low purpose of detection limit.
In order to achieve the above objectives, technical scheme is as follows：
The assay method of BAC and DDAC in a kind of soil and plant-derived product, using liquid chromatography tandem mass spectrometry, packet
Extraction, purification, three step of examination with computer are included, specific following steps are as follows：
1) it extracts, weighs sample in 50mL plastic centrifuge tubes, 5-20mL water is added, 5-20mL first is added in vortex mixing
Saturated nacl aqueous solution is added in alcohol, vortex mixing, ultrasound, and centrifugation takes supernatant, is repeated once, and merges supernatant, to be clean；
2) it purifies, pipettes above-mentioned supernatant, cross SPE purification pipes, purify and 50-500mgGCB powder, 50- are added in pipe
500mgC18 powder and 50-500mgPSA powder, be fully vortexed mixing, and centrifugation obtains second of supernatant；
3) examination with computer takes second of supernatant, nitrogen to be blown to dry, addition 1mL water redissolution, excessively film, for liquid chromatography tandem
Mass spectrograph measures.
Preferably, the chromatographic column of the Liquid Chromatography-Tandem Mass Spectrometry instrument in the liquid chromatography tandem mass spectrometry is C18,3.5 μ
M, size are 150mm × 2.1mm.
Preferably, the mobile phase of the Liquid Chromatography-Tandem Mass Spectrometry instrument is：A：0.05% aqueous formic acid, B：Acetonitrile is molten
Liquid, flow velocity 0.4mL/min, column temperature are 35 DEG C, and sample size is 2 μ L.
Preferably, the Mass Spectrometry Conditions of the Liquid Chromatography-Tandem Mass Spectrometry instrument are：A) ion source：Electric spray ion source；B) it sweeps
Retouch mode：Cation scans；C) detection mode：More reaction detections；D) dry temperature degree：400℃；E) dry gas stream speed：12L/
min；F) sheath temperature degree：350℃；G) sheath gas：12L/min；H) voltage of transfer capillary：4000V；I) atomizer pressure
Power：45psi.
Through the above technical solutions, in a kind of soil provided by the invention and plant-derived product BAC and DDAC measurement
Method, be homogenized, extracted with methanol, saltoutd, centrifuged, take supernatant, through SPE purification, concentration, for High Performance Liquid Chromatography/Mass Spectrometry/
Mass spectrograph is tested, while disposably can effectively detect 9 kinds of different compound residuals, and detection sensitivity is high, and detection limit is low, inspection
Rising limit can reach 0.010mg/kg.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below.
The assay method of BAC and DDAC in a kind of soil provided by the invention and plant-derived product, using liquid chromatogram
Tandem mass spectrometry, including extraction, purification, three step of examination with computer, specific following steps are as follows：
1) it extracts, weighs sample in 50mL plastic centrifuge tubes, 5-20mL water is added, 5-20mL first is added in vortex mixing
Saturated nacl aqueous solution is added in alcohol, vortex mixing, ultrasound, and centrifugation takes supernatant, is repeated once, and merges supernatant, to be clean；
2) it purifies, pipettes above-mentioned supernatant, cross SPE purification pipes, purify and 50-500mgGCB powder, 50- are added in pipe
500mgC18 powder and 50-500mgPSA powder, be fully vortexed mixing, and centrifugation obtains second of supernatant；
3) examination with computer takes second of supernatant, nitrogen to be blown to dry, addition 1mL water redissolution, excessively film, for liquid chromatography tandem
Mass spectrograph measures.
The chromatographic column of Liquid Chromatography-Tandem Mass Spectrometry instrument in the liquid chromatography tandem mass spectrometry be C18,3.5 μm, ruler
Very little is 150mm × 2.1mm, and mobile phase is：A：0.05% aqueous formic acid, B：Acetonitrile solution, flow velocity 0.4mL/min, column
Temperature is 35 DEG C, and sample size is 2 μ L, referring to 1 condition of gradient elution of table：
Referring to table 1：
| Time/min | A | B |
| 0-2 | 95 | 5 |
| 2.5-10 | 60 | 40 |
| 10.1-25 | 5 | 95 |
| 25.01-30 | 95 | 5 |
The Mass Spectrometry Conditions of Liquid Chromatography-Tandem Mass Spectrometry instrument are：A) ion source：Electric spray ion source；B) scan mode：Just from
Son scanning；C) detection mode：More reaction detections；D) dry temperature degree：400℃；E) dry gas stream speed：12L/min；F) sheath gas
Temperature：350℃；G) sheath gas：12L/min；H) voltage of transfer capillary：4000V；I) nebulizer pressure：45psi.
The assay method of BAC and DDAC in a kind of soil disclosed by the invention and plant-derived product with methanol homogenate, carries
It takes, saltout, centrifuging, taking supernatant, through SPE purifications, concentration, being tested for High Performance Liquid Chromatography/Mass Spectrometry/mass spectrograph, while primary
Property can effectively detect 9 kinds of different compounds residuals, detection sensitivity is high, and detection limit is low, and detection limit can reach
0.010mg/kg。
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest range caused.
Claims (4)
1. the assay method of BAC and DDAC in a kind of soil and plant-derived product, using liquid chromatography tandem mass spectrometry, including
Extraction, purification, three step of examination with computer, which is characterized in that specific following steps are as follows：
1) it extracts, weighs sample in 50mL plastic centrifuge tubes, 5-20mL water is added, 5-20mL methanol, whirlpool is added in vortex mixing
Mixing is revolved, saturated nacl aqueous solution is added in ultrasound, and centrifugation takes supernatant, is repeated once, and merges supernatant, to be clean；
2) it purifies, pipettes above-mentioned supernatant, cross SPE purification pipes, purify and 50-500mgGCB powder, 50-500mgC18 are added in pipe
Powder and 50-500mgPSA powder, be fully vortexed mixing, and centrifugation obtains second of supernatant；
3) examination with computer takes second of supernatant, nitrogen to be blown to dry, addition 1mL water redissolution, excessively film, for Liquid Chromatography-Tandem Mass Spectrometry
Instrument measures.
2. the assay method of BAC and DDAC, feature exist in a kind of soil according to claim 1 and plant-derived product
It is C18 in the chromatographic column of, the Liquid Chromatography-Tandem Mass Spectrometry instrument in the liquid chromatography tandem mass spectrometry, 3.5 μm, size is
150mm×2.1mm。
3. the assay method of BAC and DDAC, feature exist in a kind of soil according to claim 2 and plant-derived product
In the mobile phase of the Liquid Chromatography-Tandem Mass Spectrometry instrument is：A：0.05% aqueous formic acid, B：Acetonitrile solution, flow velocity are
0.4mL/min, column temperature are 35 DEG C, and sample size is 2 μ L.
4. the assay method of BAC and DDAC, feature exist in a kind of soil according to claim 3 and plant-derived product
In the Mass Spectrometry Conditions of the Liquid Chromatography-Tandem Mass Spectrometry instrument are：A) ion source：Electric spray ion source；B) scan mode：Cation
Scanning；C) detection mode：More reaction detections；D) dry temperature degree：400℃；E) dry gas stream speed：12L/min；F) sheath temperature
Degree：350℃；G) sheath gas：12L/min；H) voltage of transfer capillary：4000V；I) nebulizer pressure：45psi.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111220736A (en) * | 2020-03-24 | 2020-06-02 | 生态环境部南京环境科学研究所 | Method for determining benzalkonium chloride in plants |
| CN111239298A (en) * | 2020-03-26 | 2020-06-05 | 生态环境部南京环境科学研究所 | Method for measuring decamethylammonium chloride in plant |
| CN111257471A (en) * | 2020-03-19 | 2020-06-09 | 生态环境部南京环境科学研究所 | Method for determining benzalkonium chloride in soil |
| CN111337591A (en) * | 2020-03-26 | 2020-06-26 | 生态环境部南京环境科学研究所 | Method for measuring decamethylammonium chloride in soil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111257471A (en) * | 2020-03-19 | 2020-06-09 | 生态环境部南京环境科学研究所 | Method for determining benzalkonium chloride in soil |
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| CN111239298A (en) * | 2020-03-26 | 2020-06-05 | 生态环境部南京环境科学研究所 | Method for measuring decamethylammonium chloride in plant |
| CN111337591A (en) * | 2020-03-26 | 2020-06-26 | 生态环境部南京环境科学研究所 | Method for measuring decamethylammonium chloride in soil |
| CN111239298B (en) * | 2020-03-26 | 2021-09-21 | 生态环境部南京环境科学研究所 | Method for measuring decamethylammonium chloride in plant |
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Application publication date: 20181019 |