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Method for detecting diethylstilbestrol hormones in liquid milk according to liquid chromatography-mass spectrometer method

A technology of diethylstilbestrol and liquid milk, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of unfavorable rapid detection and long time-consuming pretreatment methods, and achieve the effect of shortening pretreatment time, reducing operation steps, and simple and fast operation

Inactive Publication Date: 2016-02-03
INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, "GB / T22992-2008 Determination of Residual Amounts of Zearalanol, Zearalane, Diethylstilbestrol, Hexestrol and Diethylstilbestrol in Milk and Milk Powder by Liquid Chromatography-Tandem Mass Spectrometry" uses liquid chromatography-mass spectrometry The method used, but its sample pretreatment method takes a long time, which is not conducive to the daily rapid detection of enterprises

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1. Experimental equipment

[0015] Ultra-high performance liquid chromatography-tandem quadrupole mass spectrometer: equipped with an electrospray ionization source (ESI) (TQD, Waters, USA) and a solid-phase extraction device (Supelco, USA).

[0016] 2. Experimental reagents and materials

[0017] Diethylstilbestrol, zearalanol, zearalane standard (Dr. Ehrenstorfer GmbH, Germany);

[0018] Methanol, acetonitrile and formic acid were all chromatographically pure;

[0019] Laboratory water is first-grade ultrapure water;

[0020] MAX solid phase extraction column (60mg / 3ml, American waters company).

[0021] 3. Solution preparation.

[0022] (1) Standard solution

[0023] Accurately weigh an appropriate amount of diethylstilbestrol, zearalanol, and zearalenone standard products, prepare a 100 mg / L standard stock solution with methanol, and store in a -18°C refrigerator. When in use, dilute with 50% acetonitrile aqueous solution as needed to make standard working sol...

Embodiment 2

[0050] On the basis of Example 1, only the sample pretreatment method is replaced as follows, and the rest of the method design is the same as that of Example 1.

[0051] Sample pretreatment method:

[0052] a. Weigh 2 g of liquid milk to be tested, add 3 mL of acetonitrile, vortex and mix for 30 seconds, then centrifuge at 5000 r / min for 5 min, pipette the supernatant to obtain supernatant A;

[0053] b. Add 2 mL of acetonitrile to the remaining precipitate, vortex and mix for 30 seconds, then centrifuge at 5000r / min for 5min, pipette the supernatant to obtain supernatant B;

[0054] c. Combine supernatant A and supernatant B, add 5mL water and mix evenly, and finally adjust the pH value to 11 with 0.1mol / L NaOH to obtain the extract;

[0055] d. Purification: take the MAX solid phase extraction column, activate and equilibrate with 4mL methanol and 4mL water in turn; take the extract obtained in step c, make it pass through the MAX solid phase extraction column, and control t...

Embodiment 3

[0057] On the basis of Example 1, only the sample pretreatment method is replaced as follows, and the rest of the method design is the same as that of Example 1.

[0058] Sample pretreatment method:

[0059] a. Weigh 2 g of liquid milk to be tested, add 3 mL of acetonitrile, vortex and mix for 40 seconds, then centrifuge at 4500 r / min for 8 min, pipette the supernatant to obtain supernatant A;

[0060] b. Add 2 mL of acetonitrile to the remaining precipitate, vortex and mix for 40 seconds, then centrifuge at 4500r / min for 8 minutes, remove the supernatant to obtain supernatant B;

[0061] c. Combine supernatant A and supernatant B, then add 5mL water and mix evenly, and finally adjust the pH value to 11.1 with 0.2mol / L NaOH to obtain the extract;

[0062] d. Purification: Take the MAX solid phase extraction column, activate and equilibrate with 5mL methanol and 5mL water in turn; take the extract obtained in step c, make it pass through the MAX solid phase extraction column, ...

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Abstract

The invention provides a method for detecting diethylstilbestrol hormones in liquid milk according to a liquid chromatograph-mass spectrometer method. A sample pretreatment method comprises the following steps: weighing 2 g of to-be-detected liquid milk, adding 3mL of acetonitrile, carrying out vortex mixing for 20-40 seconds, carrying out centrifugation at 4000-5000 r / min for 3-8 min, and transferring the supernate A, so as to obtain the supernate A; adding 2 mL of acetonitrile into the remaining precipitate, carrying out vortex mixing for 20-40 seconds, carrying out centrifugation at 4000-5000 r / min for 3-8 min, and transferring the supernate B, so as to obtain the supernate B; combining the supernate A and the supernate B, and then adding 5 mL of water for uniform mixing; finally, adjusting the pH value of the obtained mixture to 10.9-11.1 by utilizing 0.1-0.2 mol / L of NaOH, so as to obtain an extraction solution; conducting solid-phase extraction column purification on the extraction solution, so as to obtain the pretreated to-be-detected liquid milk. The method is simple and quick to operate, and both the detection and the recovery rate can meet the detection requirements.

Description

technical field [0001] The invention relates to a method for detecting hormones in milk, which is especially suitable for detecting diethylstilbestrol hormones in liquid milk by liquid mass spectrometry. Background technique [0002] Diethylstilbestrol, zearalanol and zearalane are all diethylstilbestrol hormones, which are synthetic non-steroidal anabolic hormones. They have been used in animal husbandry to improve feed conversion rate and promote livestock growth. In order to prevent these hormones from entering the human body with animal products and endangering human health; therefore, the detection method of such compounds has become a prerequisite for solving this problem. [0003] At present, methods for detecting diethylstilbestrol hormones include spectrophotometry, enzyme-linked immunoassay, gas chromatography-tandem mass spectrometry, high performance liquid chromatography, and liquid chromatography-tandem mass spectrometry. In recent years, due to the high sensi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
Inventor 崔向云张雪峰李照袁凤琴徐向峰常建军宋晓东
Owner INNER MONGOLIA MENGNIU DAIRY IND (GRP) CO LTD
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