Method for detecting 4 types of barbiturate sedatives in raw milk

A technology of barbiturates and fresh milk, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of barbiturate sedative drugs and other problems, and achieve low cost, good repetition rate and recovery rate, and high sensitivity Effect

Active Publication Date: 2017-09-26
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the above-mentioned technical problems in the prior art, the present invention provides a method for detecting 4 kinds of barbiturate sedatives in raw milk, and the met

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  • Method for detecting 4 types of barbiturate sedatives in raw milk
  • Method for detecting 4 types of barbiturate sedatives in raw milk
  • Method for detecting 4 types of barbiturate sedatives in raw milk

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Preparation of standard curve

[0060] Phenobarbital, pentobarbital, amobarbital and secobarbital were prepared into 10 μg / mL stock solutions with methanol and stored at -20°C. Before use, draw 1 mL accurately, prepare 10 mL of mixed standard solution with a concentration of 1 μg / mL with methanol, and store at -20 °C. Before use, weigh 0 μL, 50 μL, 100 μL, 200 μL, 500 μL, 1000 μL mixed standard solution, blow dry with nitrogen at 50 °C, and dilute to volume with 1 mL of blank fresh milk sample extract. Injection detection, the preparation of the standard curve.

[0061] Chromatographic column: ACQUITY CSH C18 (2.1×100mm, 1.7μm);

[0062] Column temperature: 25°C;

[0063] The flow rate is 0.3mL / min;

[0064] Injection volume: 5 μL;

[0065] Mobile phase A: water;

[0066] Mobile phase B: acetonitrile;

[0067] Gradient elution conditions are shown in Table 1

[0068] Table 1 Liquid chromatography linear gradient elution conditions

[0069] time (min) ...

Embodiment 2

[0086] Pretreatment of samples to be tested

[0087] (1) Put 10.0g of fresh milk (Ranch A) into a 50mL polypropylene centrifuge tube, add 20mL of 0.1% acetic acid acetonitrile solution, shake for 30s, and sonicate for 20min; add 2g of anhydrous sodium chloride, shake for 3min; 5000rpm, Centrifuge for 5 min; take 10 mL of the supernatant in a 15 mL polypropylene centrifuge tube, blow dry with nitrogen at 50°C, and dilute to volume with 2 mL of 30% acetonitrile aqueous solution for purification.

[0088] (2) Pass the above constant volume solution through the SPE cartridge. Pre-treat with 5 mL of methanol and 5 mL of 30% acetonitrile in water. The above-mentioned constant volume solution is passed through the column, and the flow rate is controlled at about 0.5mL / min. Then wash the column with 5mL of ultrapure water and dry it in vacuum for 15min; elute with 10mL of dichloromethane, collect the eluent, and dry it with nitrogen at 50°C; HPLC-MS / MS analysis.

[0089] The detec...

Embodiment 3

[0091] Pretreatment of samples to be tested

[0092] (1) Put 10.0g of raw milk (Ranch B) into a 50mL polypropylene centrifuge tube, add 20mL of 0.1% acetic acid acetonitrile solution, shake for 1min, and ultrasonic for 30min; add 5g of anhydrous sodium chloride, shake for 3min; 8000rpm, Centrifuge for 10 min; take 10 mL of the supernatant in a 15 mL polypropylene centrifuge tube, blow dry with nitrogen at 50°C, and dilute to volume with 2 mL of 30% acetonitrile aqueous solution for purification.

[0093] (2) Pass the above constant volume solution through the SPE cartridge. Pre-treat with 8 mL of methanol and 8 mL of 30% acetonitrile in water. The above-mentioned constant volume solution is passed through the column, and the flow rate is controlled at about 0.5mL / min. Then wash the column with 8 mL of ultrapure water, and vacuum dry it for 15 min; elute with 20 mL of dichloromethane, collect the eluate, and dry it with nitrogen at 50 ° C; HPLC-MS / MS analysis.

[0094] The ...

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Abstract

The invention discloses a method for detecting 4 types of barbiturate sedatives in raw milk. The method comprises the following steps: mixing, shaking and performing ultrasound on raw milk to be detected and acetonitrile solution, adding inorganic salt A, and performing centrifugation; drying supernatant through nitrogen gas, and fixing the volume through acetonitrile aqueous solution, so as to purify the supernatant; ensuring that acid is formic acid or acetic acid; prewashing a column through methanol and acetonitrile aqueous solution, performing column chromatography isolation on the solution to be purified, with constant volume, washing the column through ultrapure water, and performing vacuum drying; performing eluting through methylene chloride, controlling the flow velocity, drying eluent through nitrogen gas, fixing the volume on the acetonitrile aqueous solution, so as to be used for a machine; performing high-efficiency liquid chromatogram-mass spectrogram combination detection and analysis on raw milk solution to be detected obtained in a pretreatment method. The pretreatment method in the detection method can effectively improve the extraction efficiency of the barbiturate sedatives in the raw milk, and can further effectively improve the recovery percent of the barbiturate sedatives in the raw milk, the method is simple, economical and reliable, the influence on the raw milk by ground substance is effectively reduced, and the sensibility, the recurrence rate and the recovery ratio are good.

Description

technical field [0001] The invention belongs to the field of food, and relates to a food safety detection method, in particular to a method for detection of four kinds of barbiturate sedative drugs in fresh milk. Background technique [0002] Barbiturates are general central depressants, including phenobarbital, pentobarbital, amobarbital, secobarbital, etc. Sedative drugs, veterinary drugs are clinically used as sedatives and chemical sedatives, which can cause similar physiological sleep, mainly manifested in the inhibition of the central nervous system, and can also inhibit the respiratory center and vasomotor center of the medulla medulla. The depth of inhibition of the central nervous system is generally proportional to the dose. A small dose acts as a sedative, a moderate dose has a hypnotic effect, and a large dose acts as an anesthetic. When the amount is large, it can also inhibit the circulatory system and the respiratory system. Overdose can easily cause acute d...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 田怀香周兴鑫陈臣何亚斌孟瑾
Owner SHANGHAI INST OF TECH
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