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Detection method for measuring the trichlorfon in meat food by liquid chromatography-tandem mass spectrometry

A technology of liquid chromatography and tandem mass spectrometry is applied in the detection field of trichlorfon in meat food by liquid chromatography tandem mass spectrometry, which can solve the problems of complicated operation steps, high detection cost, poor sensitivity, etc. High sensitivity and good accuracy

Inactive Publication Date: 2019-05-03
厦门泓益检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Trichlorfon can be used to prevent and control internal and external parasites in pigs. It is a good multi-effect insect repellent. Trichlorfon has contact killing, stomach poisoning and osmotic activity. The residual trichlorfon in pork will pass through the digestive tract and respiratory tract and skin contact and other ways to invade the human body, thereby causing damage to people's health. Currently, the detection techniques for trichlorfon include gas chromatography, liquid chromatography, and gas chromatography tandem mass spectrometry (GC-MS), etc. The operation steps of these methods Complex, high detection cost and poor detection sensitivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: a liquid chromatography tandem mass spectrometry method for detecting trichlorfon in meat food, comprising the following steps:

[0026] Step 1: Pork sample pretreatment

[0027] 1) Use an electronic scale to weigh a 4g pork sample, and place the pork sample in a beaker;

[0028] 2) Add 30 mL of ethyl acetate to the beaker, use a homogenizer to make it fully mixed, and then sonicate in a water bath at room temperature for 10 min.

[0029] Step 2: Concentration and purification

[0030] 1) Transfer the ethyl acetate extract of the pork sample to a centrifuge tube, centrifuge for 5 minutes, and control the centrifugal speed at 8000r / min to obtain the extract;

[0031] 2) After the combined ethyl acetate extract was concentrated on a rotary evaporator, 2 mL of n-hexane and acetonitrile were added to dissolve in a 2:1 solution;

[0032] 3) Take the acetonitrile layer, pass it through a 0.22 μm filter membrane, and use it as the solution to be tested.

[00...

Embodiment 2

[0039] Embodiment 2: A liquid chromatography tandem mass spectrometry method for detecting trichlorfon in meat food, comprising the following steps:

[0040] Step 1: Pork sample pretreatment

[0041] 1) Use an electronic scale to weigh a 6g pork sample, and place the pork sample in a beaker;

[0042] 2) Add 50 mL of ethyl acetate to the beaker, use a homogenizer to make it fully mixed, and then ultrasonicate for 20 min in a water bath at room temperature.

[0043] Step 2: Concentration and purification

[0044] 1) Transfer the ethyl acetate extract of the pork sample to a centrifuge tube, centrifuge for 6 minutes, and control the centrifugal speed at 90000r / min to obtain the extract;

[0045] 2) After the combined ethyl acetate extract was concentrated on a rotary evaporator, 10 mL of n-hexane and acetonitrile were added to dissolve in a 2:1 solution;

[0046] 3) Take the acetonitrile layer, pass it through a 0.22 μm filter membrane, and use it as the solution to be tested....

Embodiment 3

[0053] Embodiment three: a liquid chromatography tandem mass spectrometry method for determining trichlorfon in meat food, comprising the following steps:

[0054] Step 1: Pork sample pretreatment

[0055] 1) Use an electronic scale to weigh a 10g pork sample, and place the pork sample in a beaker;

[0056] 2) Add 100 mL of ethyl acetate to the beaker, use a homogenizer to make it fully mixed, and then sonicate in a water bath at room temperature for 15 minutes.

[0057] Step 2: Solid Phase Extraction

[0058] 1) Transfer the ethyl acetate extract of the pork sample to a centrifuge tube, centrifuge for 10 minutes, and control the centrifugal speed at 10000r / min to obtain the extract;

[0059] 2) After the combined ethyl acetate extract was concentrated on a rotary evaporator, 6 mL of n-hexane and acetonitrile were added to dissolve in a 2:1 solution;

[0060] 3) Take the acetonitrile layer, pass it through a 0.22 μm filter membrane, and use it as the solution to be tested. ...

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Abstract

The invention, which relates to the technical field of food detection, discloses a detection method for measuring the trichlorfon in meat food by liquid chromatography-tandem mass spectrometry. The method comprises: 2g to 10g of pork samples are weighed by using an electronic scale, the pork samples are placed in a beaker, 30mL to 100mL of ethyl acetate is added into the beaker, the samples and the ethyl acetate are mixed uniformly by using a homogenizer, and then ultrasonic processing is carried out for 10 min to 20 min in normal temperature water bath; the ethyl acetate extract of the pork samples is transferred to a separating funnel, centrifugal processing is carried out for 5 to 10min in a centrifuge tube at a centrifugal speed that is controlled to be 8000-10000r / min, so that an extract is obtained. According to the invention, the trichlorfon in the port is detected by using the liquid chromatography tandem mass spectrometry and the separation ability of chromatography is combined with the qualitative function of mass spectrometry, thereby realizing the accurate quantitative and qualitative analysis of trichlorfon in pork food. In detection of the trichlorfon residues in porkfood, the interference can be effectively eliminated and the stability of a to-be-tested object can be ensured. Moreover, the detection and analysis method has high sensitivity and high accuracy.

Description

technical field [0001] The invention relates to the technical field of food detection, in particular to a liquid chromatography tandem mass spectrometry method for detecting trichlorfon in meat food. Background technique [0002] Trichlorfon belongs to the phosphate type of organophosphorus pesticides. The compound in which the hydroxyl group in the phosphoric acid molecule is replaced by an organic group to form a phosphorus-carbon bond becomes phosphoric acid, and the phosphoric acid is esterified to become a phosphoric acid ester. The allowable daily intake is 0.01mg / (kg.d) as an organophosphorus pesticide, which is easy to decompose under alkaline conditions and loses toxicity. It is relatively stable in acidic and neutral solutions, but trichlorfon decomposes under alkaline conditions The product of dichlorvos, its toxicity increased by 10 times. Its toxicity is mainly acute poisoning, and chronic poisoning is less. [0003] Trichlorfon can be used to prevent and con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 孙丽香赵叶祺邹明宇
Owner 厦门泓益检测有限公司
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