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A method for the determination of Ningnanmycin content in tomato by ultra-high performance liquid chromatography tandem mass spectrometry

A technology of ultra-high performance liquid phase and Ningnanmycin, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as matrix interference, achieve high accuracy, simple processing methods, and improve sensitivity

Active Publication Date: 2021-03-23
AGRI PRODS PROCESSING RES INST CHINESE ACAD OF TROPICAL AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the deficiencies in the prior art, the present invention provides an ultra-high performance liquid chromatography tandem mass spectrometry detection method for determining the content of Ningnanmycin in tomatoes, which uses fewer reagents and saves costs; the sample pretreatment method is simple and the purification effect Well, the technical problem of serious matrix interference is solved; the sensitivity of the detection method is greatly improved by using tandem mass spectrometry detection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] An ultra-high performance liquid chromatography tandem mass spectrometry detection method for Ningnanmycin content in tomato, comprising the following steps:

[0023] (1) Prepare the standard working solution: Weigh 0.005g of Ningnanmycin standard product into a 100mL volumetric flask, dissolve it with methanol and constant volume, then dilute with methanol and finally prepare 5 standard working solutions with concentration gradients;

[0024] (2) Extract the sample: Weigh 2.00g tomato sample and add it to a 50mL stoppered centrifuge tube, add 4g NaCl, 20mL0.1% acetic acid acetonitrile, vortex and shake for 2min, then centrifuge in a high-speed centrifuge at a speed of 5000 r / min 8min;

[0025] (3) Purify the sample: Add 100-400mg PSA, 100-300mg C18, 50-100mg GCB, 30-70mg anhydrous magnesium sulfate to a 50mL centrifuge tube respectively, take out 10 mL of the supernatant into the centrifuge tube, vortex Spin for 2min, centrifuge at 5000r / min for 3min, take out 2mL of ...

Embodiment 2

[0033] An ultra-high performance liquid chromatography tandem mass spectrometry detection method for Ningnanmycin content in tomato, comprising the following steps:

[0034] (1) Prepare the standard working solution: Weigh 0.0125g of Ningnanmycin standard product into a 100mL volumetric flask, dissolve it with methanol and constant volume, then dilute with methanol and finally prepare 5 standard working solutions with concentration gradients;

[0035] (2) Sample extraction: Weigh 3.5 tomato samples into a 50mL stoppered centrifuge tube, add 5.5g NaCl, 22.5mL 0.1% acetic acid acetonitrile, vortex and shake for 2.5min, then place in a high-speed centrifuge at 6000 r / min Speed ​​centrifugation for 9 minutes;

[0036] (3) Purify the sample: Add 100-400mg PSA, 100-300mg C18, 50-100mg GCB, 30-70mg anhydrous magnesium sulfate to a 50mL centrifuge tube respectively, take out 10 mL of the supernatant into the centrifuge tube, vortex Spin for 3.5min, centrifuge at 6500r / min for 4min, t...

Embodiment 3

[0044] An ultra-high performance liquid chromatography tandem mass spectrometry detection method for Ningnanmycin content in tomato, comprising the following steps:

[0045] (1) Prepare the standard working solution: Weigh 0.02g of Ningnanmycin standard product into a 100mL volumetric flask, dissolve it with methanol and make it to volume, then dilute with methanol and finally prepare 5 standard working solutions with concentration gradients;

[0046] (2) Extract the sample: Weigh 5.00g tomato sample and add it to a 50mL stoppered centrifuge tube, add 4-7g NaCl, 25mL0.1% acetic acid acetonitrile, vortex and shake for 3min, then place in a high-speed centrifuge at 7000 r / min Speed ​​centrifugation for 8 to 10 minutes;

[0047] (3) Purify the sample: Add 100-400mg PSA, 100-300mg C18, 50-100mg GCB, 30-70mg anhydrous magnesium sulfate to a 50mL centrifuge tube respectively, take out 10 mL of the supernatant into the centrifuge tube, vortex Spin for 5 min, centrifuge at 8000 r / min...

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Abstract

The invention relates to an ultra-high performance liquid chromatography tandem mass spectrum detection method for determining the content of ningnanmycin in tomatoes, belonging to the technical fieldof detection of pesticide residues. The method comprises the steps of carrying out vortex vibration extraction on a sample through acetonitrile, purifying by virtue of PSA, C18, GCB, anhydrous magnesium sulfate and the like, filtering purified liquid through a filtering film, separating the purified liquid by virtue of ultra-high performance liquid chromatography, detecting by virtue of tandem mass spectrum, and carrying out quantification by virtue of an external standard method. The method has the beneficial effects that adopted reagents are few, so that the cost is saved; a sample pretreatment method is simple and has a good purifying effect, so that the technical problem that the matrix interference is relatively serious is solved; by utilizing liquid phase tandem mass spectrum detection, the method has the advantages of high detection sensitivity and accuracy, good repeatability, high detection specificity and the like, and the reference is provided for the detection of the content of ningnanmycin in the tomatoes.

Description

technical field [0001] The invention relates to a detection method for Ningnanmycin content, in particular to an ultra-high performance liquid chromatography tandem mass spectrometry detection method for determining Ningnanmycin content in tomato, and belongs to the technical field of pesticide residue detection. Background technique [0002] Ningnanmycin is a cytosine nucleoside peptide type antibiotic, which is an antibiotic pesticide produced by the fermentation of Streptomyces noursii Xichang variety. 16H25N7O8. Ningnanmycin is a low-toxic antibiotic fungicide, with acute oral LD50 of 5492-6845 mg / kg for mice and mice, and acute percutaneous LD50 of mice > 1000 mg / kg, without carcinogenic, teratogenic or mutagenic effects , without accumulation. The antibiotic is widely used due to its low toxicity, low residue, no "three causes" and accumulation problems, and no environmental pollution. It has certain effects on disease prevention and production increase, and is a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 查玉兵杨春亮叶剑芝林玲
Owner AGRI PRODS PROCESSING RES INST CHINESE ACAD OF TROPICAL AGRI SCI