Method for detecting locoweed extractive and content of swainsonine in capsule

A technology of swainsonine and extract, which is applied in the field of analytical chemistry, can solve the problems of lack of chromophores, unsuitable for drug analysis, and high detection limit, and achieves a reliable analytical method, convenient and fast pretreatment process and high sensitivity. Effect

Inactive Publication Date: 2015-10-14
成霈 +1
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Due to the strong water solubility of swainsonine and the lack of chromophores suitable for spectrophotometric d

Method used

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  • Method for detecting locoweed extractive and content of swainsonine in capsule
  • Method for detecting locoweed extractive and content of swainsonine in capsule
  • Method for detecting locoweed extractive and content of swainsonine in capsule

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: the drafting of swainsonine standard curve

[0032] 1) Preparation of SW standard solution: Accurately weigh SW standard product (purity ≥ 98%), and make 1mg L with methanol -1 standard stock solution, and then diluted step by step with 1% formic acid methanol solution to 1.0, 2.5, 5.0, 10.0, 25.0, 50.0ug·L -1 standard liquid series.

[0033] 2) Experimental equipment and chromatographic conditions: Shimadzu 20A-AB3200 liquid chromatography-mass spectrometry instrument, equipped with low-pressure quaternary pump, column oven, CAPCELL PAK C18MG, specification: 5.0um, 3.0mm×150mm, chromatographic column, MultiQuant mass spectrometry operating system. The mobile phase was gradient elution of 1% formic acid and methanol by volume, the gradient program is shown in Table 1, the injection volume was 10uL, and the column temperature was 35°C. Ion source: ESI + ; Detection method: MRM; Electrospray voltage: 5.5kv; Air curtain gas flow: 10L h -1 ;Spray gas flow...

Embodiment 2

[0035] Embodiment 2: the detection of locoweed extract sample

[0036] 1) Sample pretreatment: Accurately weigh 0.001g of locoweed extract sample and place it in a 100mL volumetric flask, add 50mL of 1% formic acid methanol solution by volume, shake and ultrasonically 30min, and then dilute to volume with 1% formic acid methanol solution by volume . The graphitized carbon solid-phase extraction column was activated with 10mL water and 1% formic acid methanol solution in volume ratio before use, and the extracted sample liquid was added to the graphitized carbon solid-phase extraction column, the first 1mL was discarded, and the subsequent filtrate 1mL was collected. The collected filtrate was diluted 1000 times with methanol step by step, and the diluted liquid was purified by a 0.22um organic needle filter and then measured on the machine. The retention time of the sample was 1.42min, and the content of swainsonine in the sample was 97.2%, see figure 2 .

[0037] 2) Experi...

Embodiment 3

[0038] Example 3: Detection of swainsonine in capsules.

[0039] 1) Pretreatment of the sample: Mix the contents of the capsule evenly, accurately weigh 0.50 g of the content and place it in a 50 mL centrifuge tube, add 10 mL of 1% formic acid methanol solution by volume, shake and ultrasonic for 30 min, then centrifuge at 4000 r min -1, 10min. The graphitized carbon solid-phase extraction column is activated with 10mL water and 1% formic acid methanol solution in volume ratio before use, and the supernatant is added to the graphitized carbon solid-phase extraction column. After purifying with an organic syringe filter, it was tested on the machine, the retention time of the sample was 1.43min, and the content of swainsonine in the sample was 8.02μg·L -1 ,See image 3 .

[0040] 2) Experimental apparatus and chromatographic conditions: with embodiment 1.

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Abstract

The invention relates to a method for detecting a locoweed extractive and a content of swainsonine in a capsule. The method comprises the following steps: 1) extracting the locoweed extractive or swainsonine in the capsule via soaking through a formic acid-methanol solution with a volume ratio of 1%; 2) purifying the extracting solution by adopting a graphitized carbon solid phase extraction column and a syringe filter; 3) separating and detecting swainsonine via adopting a high performance liquid chromatogram-mass spectrometer (HPLC-MS); and 4) plotting swainsonine with different concentrations and corresponding peak areas to obtain a standard curve of swainsonine. The content of swainsonine is calculated by contrasting the peak area of a to-be-detected sample with the standard curve. The HPLC-MS is extremely high in sensitivity, is free of most matrix interference, and is more convenient and efficient in pre-treatment process, and accurate and reliable in detection result, compared with other detection methods. The method is high in sensitivity and good in specificity and reproducibility, and is a reliable analytical method.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, in particular to a method for detecting the content of swainsonine in locoweed extracts and capsules. Background technique [0002] Locoweed is the general term for the poisonous plants of the genus Oxytropis and Astragalas in the leguminous family, and it is one of the most widely distributed poisonous plants in my country and the western United States. According to incomplete statistics, there are 44 species of locoweeds in my country (including 21 species of milk vetch and 23 species of Oxytropis genus), and 15 species that pose serious hazards (including 6 species of milk vetch and 9 species of Oxytropis genus) , mainly distributed in Shaanxi, Gansu, Qinghai, Tibet, Xinjiang, Inner Mongolia, Shanxi, Ningxia, Sichuan and other provinces. Locoweeds endanger the safety of herbivores, and after livestock eat locoweeds, it can lead to locoweed poisoning syndrome. [0003] Swainsonine...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 成霈
Owner 成霈
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