Method for simultaneously detecting laxative components in weight-losing product based on UPLC-MS/MS

A detection method and component technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of poor reproducibility, complicated steps, insufficient matrix, etc., and achieve the effect of small recovery loss, good filtration effect, and simple steps

Pending Publication Date: 2021-11-09
厦门泓益检测有限公司 +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Abuse of laxatives can lead to dehydration, poisoning, miscarriage, hemorrhage, etc., which can lead to life-threatening in severe cases
[0004] At present, the analysis of laxative ingredients in food mainly includes liquid phase method, liquid chromatography mass spectrometry, etc. For example, the "Working Regulations on Food Supplement Inspection Methods" BJS201710 stipulates the detection method of phenolphthalein, and BJS201911 stipulates the detection method of sodium picosulfate. SN / T3866-2014 detects phenolphthalein and emodin at the same time. However, the existing standard and literature methods can analyze not many types of drugs at the same time, and the matrix of health care preparations covered is insufficient. The steps are complicated, the accuracy is low, and the reproducibility is low. Poor, it is difficult to quickly conduct qualitative and quantitative analysis on multiple types of illegally added laxatives in weight loss products

Method used

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  • Method for simultaneously detecting laxative components in weight-losing product based on UPLC-MS/MS
  • Method for simultaneously detecting laxative components in weight-losing product based on UPLC-MS/MS
  • Method for simultaneously detecting laxative components in weight-losing product based on UPLC-MS/MS

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Experimental program
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Effect test

Embodiment 1

[0031] refer to figure 1 As shown, the present invention discloses a method for simultaneous detection of laxative ingredients in weight loss products based on UPLC-MS / MS. The laxative ingredients include 8 ingredients, namely phenolphthalein, emodin, sodium picosulfate, bisacodyl, diacetate phenbutanol, sennoside A, sennoside B and aloin, and the simultaneous detection method includes the following steps:

[0032] S1. Preparation of standard products: Weigh the standard products of 8 kinds of laxative ingredients, weigh 10 mg, place them in 10 mL volumetric flasks, add methanol solution to dissolve and dilute to volume, and obtain a single standard stock solution.

[0033] S2. Preparation of standard solution: pipette the single standard stock solution in step S1 respectively, add methanol solution to dilute and prepare a mixed standard solution with a concentration of 100 ng / mL.

[0034] S3. Sample pretreatment: Weigh samples from weight loss products and place them in a 50...

Embodiment 2

[0055] The preparation of standard products, preparation of standard solutions, sample pretreatment, and on-machine detection and analysis steps in this embodiment are the same as those in Example 1. This embodiment adopts the external standard method for quantification, which is used to obtain the detection limit and quantification limit of the laxative components.

[0056] The linear range of the concentration of bisacodyl in the detection items of laxative ingredients is set at 0.5-10ng / mL, and the other phenolphthalein, emodin, sodium picosulfate, diacetate, sennoside A, sennoside B and aloin The linear range of the concentration of the project is set at 5-100ng / mL, and the correlation coefficient R of the curve equation within the concentration range 2 >99, with a good linear relationship; the lower limit of detection of the corresponding concentration was obtained when the signal-to-noise ratio was 3 times, and the lower limit of quantification of the corresponding concen...

Embodiment 3

[0062] In this embodiment, the configuration standard product, configuration standard solution, sample pretreatment and on-machine detection and analysis steps are the same as in Embodiment 1. The samples in this embodiment are undetected tablets, capsules or liquid weight loss products based on the pre-test results. Base, spiked at two levels of low concentration and high concentration, respectively, where the added concentrations of bisacodyl were 0.2 μg / kg and 1.0 μg / kg, and the added concentrations of other laxative ingredients were 2 μg / kg and 10 μg / kg , and do parallel tests (n=6) at the same time to obtain the recovery rate and RSD of the laxative components of different bases; the recovery rate of standard addition=(measured value of the added standard sample-measured value of the sample) / amount of added standard×100%; The recoveries and RSDs of the laxative ingredients are shown in Table 4.

[0063] The standard recovery rate and RSD of table 4 laxative composition

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Abstract

The invention discloses a method for simultaneously detecting laxative components in a weight-losing product based on UPLC-MS / MS. The method comprises the following steps of: weighing standard substances of eight laxative components, respectively putting the standard substances into volumetric flasks, adding a methanol solution, dissolving, diluting and fixing the volume to obtain single standard stock solutions; respectively transferring the single standard stock solutions, and adding a methanol solution for dilution to prepare a mixed standard solution; weighing a sample from a weight-losing product, placing the sample in a centrifuge tube, adding a methanol solution, mixing well by vortex, collecting a supernatant through ultrasonic extraction and centrifugation, extracting the supernatant, carrying out nitrogen blowing concentration until the supernatant is nearly dry, adding methanol water for redissolving, and filtering through a filter membrane to obtain a sample to be detected; and respectively performing qualitative and quantitative analysis and determination on the mixed standard solution and the sample to be detected by using an ultra-high performance liquid chromatography-tandem mass spectrometer to obtain the types and contents of the laxative components in the sample. The method can be used for simultaneously carrying out qualitative and quantitative analysis on various laxative components, and has the advantages of simple steps, high accuracy and good reproducibility.

Description

technical field [0001] The invention relates to the technical field of health care products, in particular to a simultaneous detection method for laxative ingredients in weight loss products based on UPLC-MS / MS. Background technique [0002] With the improvement of people's living standards, obesity has become a health problem that people pay more and more attention to. Modern medicine has proved that obesity will increase people's risk of cardiovascular and cerebrovascular diseases, digestive system diseases and endocrine system diseases, and may even induce dictation cancer. Obesity has brought huge hidden dangers to people's health, and it has also caused an increasingly heavy burden on the public health systems of various countries. The huge demand for weight loss has given birth to the weight loss health food market, and products such as weight loss coffee, weight loss tea, weight loss capsules, weight loss biscuits, and weight loss enzymes emerge in endlessly. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/34G01N30/7233G01N30/8679
Inventor 洪家俊邹明宇杨旺火
Owner 厦门泓益检测有限公司
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