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Method for rapidly detecting clenbuterol hydrochloride with solid phase microextraction and gas chromatography-mass spectrometry technique

A technology of clenbuterol hydrochloride and gas chromatography mass spectrometry, which is applied in the field of fast detection of clenbuterol hydrochloride by solid-phase microextraction and gas chromatography mass spectrometry, can solve the problem of unfriendly organic solvent environment, high cost and pretreatment method Time-consuming and other problems, to achieve the effect of simple and convenient operation, low cost, good promotion and application value

Inactive Publication Date: 2014-05-28
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the technical deficiencies of the existing clenbuterol hydrochloride standard detection method sample pretreatment method, such as time-consuming, high cost, and a large amount of organic solvents that are not friendly to the environment, and provide a fast, accurate, environmentally friendly, low-cost Cost-effective method for the detection of clenbuterol hydrochloride

Method used

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  • Method for rapidly detecting clenbuterol hydrochloride with solid phase microextraction and gas chromatography-mass spectrometry technique
  • Method for rapidly detecting clenbuterol hydrochloride with solid phase microextraction and gas chromatography-mass spectrometry technique
  • Method for rapidly detecting clenbuterol hydrochloride with solid phase microextraction and gas chromatography-mass spectrometry technique

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Experimental program
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Effect test

Embodiment 1

[0041] The preparation of embodiment 1 detachable solid-phase microextraction (SPME) probe

[0042] The preparation method of detachable solid-phase microextraction (SPME) probe of the present invention is as follows:

[0043] S1. Cut the stainless steel wire into a section of 3-4cm, and cut the polydimethylsiloxane (PDMS) tube into a section of 1cm;

[0044] S2. The stainless steel wire cut by S1 is ultrasonically cleaned with ultrapure water and acetone for 10 minutes, and dried for later use;

[0045]S3. Take the same amount of glue A and glue B of high-temperature epoxy resin glue, mix well, apply the mixed glue thinly and evenly on the surface of the treated stainless steel wire, and then cover it with a cut 1cm polydimethylsiloxane Alkane (PDMS) tube, let the glue cure naturally at room temperature, and get the extraction coating;

[0046] S4. Place the extraction coating at 250° C., and age it in a nitrogen flow for 30 minutes to remove impurities on the extraction co...

Embodiment 2

[0049] Example 2 GC-MS sample injection experiment of clenbuterol hydrochloride derivative standard solution

[0050] 1. Preparation of clenbuterol hydrochloride standard solution

[0051] S1. Weigh 0.010g of clenbuterol hydrochloride into a 20mL brown bottle, dilute with methanol to the mark on the bottle, shake well, make a 500mg / L stock solution, and store in a refrigerator at 4°C;

[0052] S2. Take an appropriate amount of the stock solution obtained from S1 in a 500mL volumetric flask, dilute it with methanol, prepare a standard solution with a concentration of 2000μg / L, 1600μg / L, and 1000μg / L, and store it in a refrigerator at 4°C;

[0053] S3. Take 1 mL of the 2000 μg / L and 1000 μg / L standard solutions obtained from S2 respectively in a 10 mL volumetric flask, dilute with methanol to prepare standard solutions with a concentration of 200 μg / L and 100 μg / L, and store them in a refrigerator at 4 °C.

[0054] 2. Preparation of standard solution of clenbuterol hydrochlorid...

Embodiment 3

[0065] Embodiment 3 detection condition optimization experiment

[0066] 1. Experimental materials

[0067] (1) Material: Purchase fresh blank lean pork, rinse the surface with tap water and grind it thoroughly with a blender.

[0068] (2) Spiked pork: Weigh 2.00 g of minced blank pork samples into 10 mL sample bottles, add 100 μL of clenbuterol hydrochloride standard solution with a concentration of 200 μg / L, and prepare the spiked pork with a concentration of 100 μg / kg. Standard pork.

[0069] 2. Extraction time optimization experiment

[0070] The 100 μg / kg spiked pork prepared above was repeated multiple times. The newly prepared and aged detachable solid-phase microextraction probe was inserted into the spiked pork, and the probes were left at room temperature for different extraction times. The needle was inserted into a 10 mL sealed sample bottle filled with 50 μL of MTBSTFA, derivatized in headspace at 50°C for 30 min, injected directly after derivatization, and ana...

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Abstract

The invention provides a method for rapidly detecting clenbuterol hydrochloride with a solid phase microextraction and gas chromatography-mass spectrometry technique. According to the method, firstly, a detachable solid phase microextraction probe is used for extracting a to-be-detected sample, then, MTBSTFA (N- tert-butyldimethylsilyl)-N- methyltrifluoroacetamide) is used for performing derivatization on an extract, finally, a gas chromatography-mass spectrometer is used for analytic determination, and an external standard method is used for quantification. The method is environment-friendly, simple and convenient to operate, time-saving and labor-saving; the detecting time is only 90 minutes, the sample pretreatment cost is lower than one yuan, and the method can be very conveniently applied to rapid screening of clenbuterol hydrochloride in various samples and has good popularization and application values.

Description

technical field [0001] The invention relates to the field of agricultural product quality detection. More specifically, it relates to a method for rapid detection of clenbuterol hydrochloride by solid phase microextraction and gas chromatography mass spectrometry. Background technique [0002] Clenbuterol hydrochloride is a synthetic stimulant that has the effect of dilating the bronchi and is often used to prevent and treat lung diseases such as asthma and emphysema. When its application dose reaches 5-10 times of the therapeutic dose, it has the effect of redistribution of energy, which can increase muscle synthesis and reduce fat deposition, so it is commonly known as "clenbuterol" in China. Because clenbuterol hydrochloride has obvious effects of promoting growth, increasing lean meat percentage and reducing fat, it is currently used in animal husbandry as clenbuterol. But clenbuterol hydrochloride has a serious impact on human health, so the detection of clenbuterol h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 欧阳钢锋叶底如吴素素朱芳
Owner SUN YAT SEN UNIV
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