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Method for detecting sodium picosulfate in food

A technology of sodium picosulfate and food, applied in measuring devices, instruments, scientific instruments, etc., to achieve the effect of wide application range and fast detection speed

Active Publication Date: 2019-06-04
广东省药品检验所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the past, the research on illegal addition detection was concentrated in the field of health products and Chinese patent medicines, and there were few detections in food. Jelly and candied fruit are easily overlooked sample types, which have strong concealment
At present, there is no method for detecting sodium picosulfate in food or health food, and it is urgent to supplement

Method used

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  • Method for detecting sodium picosulfate in food
  • Method for detecting sodium picosulfate in food
  • Method for detecting sodium picosulfate in food

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0077] 4. Preparation of sample solution

[0078] 1. Extraction

[0079] Jelly sample: Weigh 1g of sample into a 50mL centrifuge tube, add 25mL of water accurately, bathe in 80°C water bath for 10min, take it out and shake gently until the jelly dissolves, and wait for purification.

[0080] Candied fruit sample: Weigh 1g sample into a 50mL centrifuge tube, add 25mL water accurately, ultrasonically extract for 15min, centrifuge at 8000r / min for 5min, and the supernatant is to be purified.

[0081] Liquid beverages and oral liquids: Weigh 1g of sample into a 50mL centrifuge tube, add 25mL of water accurately, bathe in 80℃ water for 10min, centrifuge at 8000r / min for 5min, and the supernatant is to be purified.

[0082] Solid beverage: Weigh 1g of sample into a 50mL centrifuge tube, add 25mL of water, bathe in 80°C for 10min, centrifuge at 8000r / min for 5min, take the supernatant, add 20mL of water to wash the residue, centrifuge at 8000r / min for 5min, combine the two extracts ...

Embodiment 1

[0092] Example 1 - Rapid Screening of Jelly Positive Samples

[0093] Weigh 1g of jelly sample into a 50mL centrifuge tube, add 25mL of water accurately, bathe in 80°C water bath for 10min, take it out and shake gently until the jelly dissolves, ready to be tested.

[0094] Take by weighing 10mg sodium picosulfate standard substance (purity 96%, Trc company), use 10mL water to prepare the standard stock solution of mass concentration 1mg / mL; Take appropriate standard stock solution, water preparation mass concentration is the detection limit of 2ng / mL solution.

[0095] Take 5 μL of the detection limit solution and the sample solution and inject them into the high-performance liquid chromatography-mass spectrometer respectively, and measure according to the following chromatography-mass spectrometry conditions.

[0096] Chromatographic conditions: chromatographic column ThermoAccucore RP-MS (100mm×2.1mm, 2.6μm, American Thermo Company); flow rate 0.3mL / min, acetonitrile: 0.01...

Embodiment 2

[0099] Embodiment 2——quantitative detection of candied fruit positive sample

[0100] Weigh 1g of chopped enzyme plum sample into a 50mL centrifuge tube, accurately add 25mL of water, ultrasonically extract for 15min, and centrifuge at 8000r / min for 5min. Take 1g of polyamide powder, activate it with 10mL of water, and fill it into a disposable syringe with an appropriate amount of cotton. Take 10mL of the extract in a syringe filled with polyamide powder. After the solution has run out, wash it with 10mL of water, 15mL of 70% methanol, and elute with 20mL of 10% ethanol ammonia solution. Collect the eluent and evaporate it on a water bath at 80°C to nearly Dry, dilute to 10mL with water, pass through a 0.22μm filter membrane, to be tested.

[0101] Weigh 10 mg of sodium picosulfate standard substance, and prepare a standard stock solution with a mass concentration of 1 mg / mL with 10 mL of water; Standard curve solution of mL, 100ng / mL, 250ng / mL, 500ng / mL, 1000ng / mL.

[010...

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Abstract

The invention discloses a method for detecting sodium picosulfate in a food. The method for detecting sodium picosulfate in the food comprises the steps that 1) a sample solution is prepared: a food sample is extracted with water to acquire the sample solution; 2) sodium picosulfate standard solutions are prepared: a sodium picosulfate standard and water are used to prepare a series of standard solutions; and 3) sample detection: the sample solution and the sodium picosulfate standard solutions are separately injected into a high performance liquid chromatography-mass spectrometer for qualitative or / and quantitative analysis. The detection method provided by the invention covers the substrate of jelly, candied fruit, solid beverage, liquid beverage and the like, has the advantages of wideapplication range and fast detection speed, and can be used as a qualitative and quantitative screening method for sodium picosulfate in the food to fill in blanks in the field of illegal addition detection.

Description

technical field [0001] The invention relates to a method for detecting illegally added chemical drugs in food, in particular to a method for detecting sodium picosulfate in food. Background technique [0002] my country has been cracking down on the illegal addition of drugs in weight loss products, but due to the variety of added drug ingredients and complex product matrices, the problem is still relatively prominent. my country's "Food Safety Law" stipulates that no drugs may be added to food. However, in order to improve the product effect, some merchants add chemical drugs to weight loss laxative food and health food. Sodium picosulfate is a new illegal added ingredient. [0003] Sodium picosulfate, also known as 4,4'-(pyridin-2-ylmethylene) bisphenyl bissulfate sodium salt, CAS No. 10040-45-6, molecular formula C 18 h 13 NNa 2 o 8 S 2 . Sodium picosulfate is a laxative that can be used for various forms of constipation. Its unilateral preparation is approved for...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/14
Inventor 何嘉雯温家欣赖宇红刘亚雄曹雅静陈余杰谭杰
Owner 广东省药品检验所
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