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Detection and analysis method of phytosterol

A phytosterol and analysis method technology, applied in the direction of analysis materials, measurement devices, material separation, etc., can solve the problems of cumbersome process, harsh reaction conditions, high reaction temperature, etc., achieve mild and rapid derivatization reaction, reduce matrix interference, and operate steps simple effect

Inactive Publication Date: 2015-01-21
QUFU NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent (CN102967647A) discloses a method of using pyridine or deuterated pyridine as a derivatization reagent and trifluoromethanesulfonic anhydride as a catalyst to detect sterol compounds in edible oil by electrospray ionization-quadrupole-time-of-flight tandem mass spectrometry. Analysis and detection have improved the detection sensitivity of sterol compounds, but the derivative reagents used in this method have a foul smell and strong irritation, and the catalyst trifluoromethanesulfonic anhydride has a strong irritating odor, which is not environmentally friendly and is harmful to the human body. Saponification after extraction is required before the derivatization reaction, the reaction conditions are harsh, the process is cumbersome, and the detection substance is a specific sample; Chinese patent (CN102978272A) synthesized phytosterol polybasic acid monoesters by using polybasic organic acids or acid anhydrides under the action of a catalyst, but the Method The reaction time is as long as 6-72 hours, the reaction temperature is high, and the energy consumption is large

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  • Detection and analysis method of phytosterol
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  • Detection and analysis method of phytosterol

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Chromatographic separation and qualitative and quantitative analysis of phytosterols by mass spectrometry:

[0043] Standard phytosterols (purchased from China Institute for the Control of Biological Products and Sigma Reagent Company) were prepared with acetonitrile to obtain a concentration of 1.0 × 10 -5 mol / L phytosterol standard solution, add 300 μ L 4'-carboxyrhodamine acetonitrile solution, 300 μL CMPI acetonitrile solution and 300 μL DMAP acetonitrile solution to the standard solution, 4'-carboxyrhodamine is dissolved in acetonitrile to obtain 1.0 × 10 -4mol / L4'-carboxyrhodamine acetonitrile solution, CMPI and DMAP were prepared into acetonitrile solutions with a mass concentration of 5% and 20%, respectively, for derivatization reaction to obtain phytosterol derivatives.

[0044] Using acidic acetonitrile / water solution (containing 0.1% formic acid) as the mobile phase, good resolution can be obtained according to the gradient elution procedure in the experim...

Embodiment 2

[0048] The detection and analysis of free phytosterols in corn oil comprises the following steps:

[0049] Take 100 μL of corn oil into a centrifuge tube and dilute to 2 mL with deionized water. Quickly inject a mixed solution containing 80 μL of chloroform and 300 μL of methanol. After ultrasonic vibration for 2 minutes, a uniform emulsion system was formed, with a pH value of 6, and centrifuged at a high speed for 3 minutes at a speed of 10,000 r / min. The organic phase was deposited at the bottom of the centrifuge tube, and the deposited phase was sucked up with a micro-syringe and transferred to another vial, dried with nitrogen and dissolved in acetonitrile. Add 300 μL of 1 × 10 -4 mol / L 4'-carboxyrhodamine acetonitrile solution, 200 μL 5w% CMPI acetonitrile solution and 200 μL 18w% DMAP acetonitrile solution, sealed and shaken well, placed in a 45 °C water bath for 30 minutes to obtain the derivatized product. The derivatized product solution was filtered through a 0.4...

Embodiment 3

[0051] The detection of free phytosterols in soybean milk includes the following steps:

[0052] Take 200 μL of soybean milk and add perchloric acid to remove protein, and dilute to 2 mL with deionized water. Quickly inject a mixed solution containing 80 μL of chloroform and 300 μL of methanol. After ultrasonic vibration for 2 minutes, a uniform emulsion system is formed, with a pH value of 6, centrifuged at a high speed for 3 minutes, and the rotation speed is 10000r / min. The organic phase was deposited at the bottom of the centrifuge tube, and the deposited phase was sucked up with a micro-syringe and transferred to another vial, dried with nitrogen and dissolved in acetonitrile. Add 200 μL of 1×10 to the vial -4 mol / L 4'-carboxyrhodamine acetonitrile solution, 200 μL 8w% CMPI acetonitrile solution and 200 μL 12w% DMAP acetonitrile solution, sealed and shaken well, placed in a 45°C water bath for 30 minutes to obtain the derivatized product. The derivatized product s...

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Abstract

The invention relates to a detection and analysis method of phytosterol. Firstly, the phytosterol is derivatized by using a derivatization reagent-4'-carboxyl rhodamine, and an ultra-high performance liquid chromatography triple quadrupole tandem mass spectrometry with a multi-reaction monitoring mode is used for carrying out qualitative and quantitative detection and analysis in the method. The method comprises the following steps: firstly, extracting the phytosterol by utilizing an ultrasonic assistance-dispersive liquid-liquid microextraction technique, then adding a 4'-carboxyl rhodamine acetonitrile solution, a 2-chlorine-1-methyl iodine pyridine acetonitrile solution and a 4-dimethyl aminopyridine acetonitrile solution into an obtained phytosterol extract for derivatization reaction, and finally analyzing and detecting by an ultra-high performance liquid chromatography triple quadrupole tandem mass spectrometry system. The method is moderate, rapid, and high in sensitivity, and has the important significance on the quality control of vegetable oil, beverages and medicinal materials which are rich in phytosterol.

Description

technical field [0001] The invention relates to a method for detecting and analyzing phytosterols, in particular to a method for detecting and analyzing phytosterols derivatized by 4'-carboxyrhodamine. Background technique [0002] Phytosterols are a class of substances with cyclopentane perhydrophenanthrene as the skeleton, which mainly exist in the roots, stems, leaves, fruits and seeds of plants. Studies in recent years have shown that phytosterols have high nutritional value and strong physiological activity. They have medicinal and health functions such as lowering blood cholesterol levels, preventing coronary atherosclerosis, anti-oxidation, and anti-cancer. They are widely used in medicine, food, cosmetics and other fields. Caused widespread concern. [0003] However, phytosterol molecules lack a chromophore or a molecular component that is sensitive to mass spectrometry, so the sensitivity of traditional UV-visible, fluorescence and mass spectrometry detection is ve...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 朱树芸赵先恩吕涛尤进茂
Owner QUFU NORMAL UNIV
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