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Method for one-time and simultaneous measurement of five preservatives in fruits

A preservative and one-time technology, applied in the field of liquid chromatography, can solve the problems of toxicity and residue, scattered measurement methods, single measurement items, etc., and achieve the effects of improving sensitivity and stability, obvious extraction effect, and accurate analysis data

Active Publication Date: 2017-12-01
PUBLIC MONITORING CENT FOR AGRO PROD OF GUANGDONG ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although chemical antiseptic preservatives have obvious inhibitory and antiseptic effects on fruit diseases, most of them have varying degrees of toxicity and residues, and they are gradually found to have adverse effects on human health during use, and even teratogenic and carcinogenic Mutagenicity has also become a very important "bottleneck" problem restricting fruit export in recent years
[0003] The detection method for fruit antiseptic and preservative residues is not yet perfect, the measurement methods are scattered, the measurement items are relatively single, and the pretreatment steps are relatively cumbersome, etc.
For example, carbendazim and thiabendazole are commonly used in liquid chromatography, prochloraz is only available in fruit gas chromatography, iprodione can be used in gas phase or liquid phase, and there is no specific standard method for the determination of imazalil in fruit

Method used

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  • Method for one-time and simultaneous measurement of five preservatives in fruits

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of standard solution: from the standard stock solution (100 mg / L) of carbendazim, thiabendazole, imazalil, iprodione and prochloraz respectively, quantitatively pipette according to the concentration value of the mixed standard solution Mix, then dilute to volume with banana blank matrix solution to obtain mixed standard solutions with mass concentrations of 0.10mg / L, 0.50mg / L, 1.00mg / L, 2.50mg / L, 5.00mg / L, and 10.0mg / L;

[0031] (2) Sample extraction: after the banana sample was sampled by quartering method, crushed with a tissue homogenizer, accurately weighed 10.0 g of the sample to be tested, put it into a 50 mL centrifuge tube, added 20 mL of acetonitrile containing 1% acetic acid, Then add 3g of sodium chloride, shake and extract for 25 minutes, and let stand for 30 minutes to separate the acetonitrile phase and the water phase;

[0032] (3) Preparation of test solution: pipette 5mL of acetonitrile extract into a coated centrifuge tube, add 100mg o...

Embodiment 2

[0053] Different from Example 1, what used in step (1) is the mixed standard solution containing citrus blank matrix; the raw material adopted in step (2) is citrus, and the citrus sample is smashed with a tissue homogenizer, and accurately weighed Put 10.0 g of the sample to be tested into a 50 mL centrifuge tube, add 20 mL of acetonitrile containing 0.6% acetic acid, then add 3.5 g of sodium chloride, extract by shaking for 30 min, and let stand for 30 min to separate the acetonitrile phase and the water phase.

[0054] When using citrus as raw material, operate according to the method of the present invention, the recovery data of the five kinds of antiseptic preservative residue detection samples in this embodiment are shown in Table 6.

[0055] The recoveries of five kinds of antiseptic preservative residue detection samples in table 6 citrus

[0056] Recovery rate

[0057] When using citrus as raw material, operate according to the method of the present inventi...

Embodiment 3

[0065] Different from Examples 1 and 2, what used in step (1) is the mixed standard solution that contains mango blank matrix; The raw material that adopts in step (2) is mango, and mango sample is smashed with tissue homogenizer, accurately Weigh 10.0 g of the sample to be tested, put it into a 50 mL centrifuge tube, add 20 mL of acetonitrile containing 0.8% acetic acid, then add 3 g of sodium chloride, extract by shaking for 30 min, and let stand for 30 min to separate the acetonitrile phase and the water phase.

[0066] When using mangoes as raw materials, operate according to the method of the present invention, the recovery data of the five kinds of antiseptic preservative residue detection samples in this embodiment are shown in Table 9.

[0067] The recoveries of five kinds of preservative preservative residue detection samples in table 9 mango

[0068] Recovery rate

[0069] When using mangoes as raw materials, operate according to the method of the present i...

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Abstract

The invention discloses a method for one-time and simultaneous measurement of five preservatives in fruits. The method includes the steps: (1) preparing mixed standard solution (substrate standard); (2) extracting samples; (3) preparing liquid to be measured; (4) measuring liquid chromatography. According to the method, pretreated extracting agents and cleaning agents are improved, a dispersion solid-phase extraction technique replaces a solid-phase extraction cartridge purification technique, computer measurement is performed by a combined organic flowing phase, a gradient elution program and a wavelength detection technique, correction is performed by the substrate standard, and the five preservatives can be rapidly and accurately measured once.

Description

technical field [0001] The invention belongs to the technical field of liquid chromatography, and in particular relates to a method for simultaneously determining five kinds of antiseptic and fresh-keeping agents in fruits at one time. Background technique [0002] Antiseptic preservatives have good antiseptic and fresh-keeping effects on post-harvest vegetables and fruits. They are widely used in post-harvest treatment and are important auxiliary means for fruit storage and preservation at home and abroad. The antiseptic preservatives used on fresh fruits in my country have a variety of trade names, but the most commonly used types are mainly benzimidazoles (thiabendazole, benomyl, carbendazim), sterols (mixian amines, biguanide salts, imazalil); formimides (iprodione), etc. Although chemical antiseptic preservatives have obvious inhibitory and antiseptic effects on fruit diseases, most of them have varying degrees of toxicity and residues, and they are gradually found to h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 邓义才骆冲黄灿亮叶倩
Owner PUBLIC MONITORING CENT FOR AGRO PROD OF GUANGDONG ACADEMY OF AGRI SCI
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