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Method and sample pretreatment method for detecting content of fat-soluble vitamins in formula milk powder

A fat-soluble vitamin and sample pretreatment technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of complex processing process and long time consumption, and achieve the effect of good repeatability, simple steps, and shortened detection cycle

Inactive Publication Date: 2018-12-18
BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECH CENT
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Zhao Kongxiang et al. (Zhao Kongxiang, Lou Tingting, He Jia, Chen Qiyong, Ge Baokun, Zheng Wenjie. Determination of fat-soluble vitamins in infant formula milk powder by isotope dilution / liquid chromatography-tandem mass spectrometry. Chinese Journal of Analysis and Testing, 2015,34(12):1372-1376. ) using isotope dilution / liquid chromatography-tandem mass spectrometry (equipped with an atmospheric pressure chemical ionization source) to simultaneously determine the fat-soluble vitamins A, D, E and K1 in infant formula milk powder, but the sample pretreatment process is relatively complicated, and the sample needs to go through Lipase hydrolysis overnight, followed by saponification reaction, petroleum ether extraction and other steps, the whole process takes a long time

Method used

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  • Method and sample pretreatment method for detecting content of fat-soluble vitamins in formula milk powder
  • Method and sample pretreatment method for detecting content of fat-soluble vitamins in formula milk powder
  • Method and sample pretreatment method for detecting content of fat-soluble vitamins in formula milk powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1. Materials and instruments

[0058] 1.1 Materials

[0059] Methanol: chromatographically pure, Fisher chemicals Inc.

[0060] Ammonium acetate: chromatographic grade, Fisher chemicals Inc.

[0061] Ethanol: analytically pure, Sinopharm Chemical Reagent Co., Ltd.

[0062] Petroleum ether: analytically pure, Sinopharm Chemical Reagent Co., Ltd.

[0063] Isopropyl ether: analytically pure, Sinopharm Chemical Reagent Co., Ltd.

[0064] Ascorbic acid: analytically pure, Sinopharm Chemical Reagent Co., Ltd.

[0065] Potassium hydroxide: analytically pure, Sinopharm Chemical Reagent Co., Ltd.

[0066] Ultrapure water: Class I water in accordance with GB / T6682.

[0067] Vitamin A, vitamin E (alpha-tocopherol), vitamin D 2 , Vitamin D 3 , vitamin K1 and other standard products were purchased from Dr.Ehrenstorfer GmbH (Ausburg, Germany); vitamins A-D 5 , Vitamin D 2 -D 3 , Vitamin D 3 -D 3 Vitamin E-D 6 , Vitamin K 1 -D 7 and other standard products were purchas...

Embodiment 2

[0120] The mensuration of embodiment 2 standard quality control milk powder sample

[0121] The infant formula quality control milk powder sample is tested, specifically through the following steps:

[0122] (a) Sample pretreatment

[0123] Accurately weigh 1.00g of formula milk powder quality control sample into a 50mL capped centrifuge tube, add 200μL of vitamin D with a concentration of 1μg / mL 2 -D 3 , Vitamin D 3 -D 3 Mix the internal standard solution and 100 μL of vitamins A-D at a concentration of 10 μg / mL 5 , Vitamin E-D 6 , Vitamin K 1 -D 7 Mix the internal standard solution, add 0.3g of ascorbic acid, 10mL of absolute ethanol and 2 mL of 60% KOH solution for saponification, cover immediately after filling with nitrogen, and vortex to mix. Shake in a constant temperature shaker at 80°C for 15 minutes, then take out the centrifuge tube and cool to room temperature; add 20 mL of n-hexane, place in the shaker for 15 minutes, take it out, add water to 50 mL, shake...

Embodiment 3

[0128] Verification of embodiment 3 detection method

[0129] 1. Linear range

[0130] Since the content of different vitamins in infant formula milk powder varies greatly, ranging from μg / 100g to mg / 100g, the requirements for detection sensitivity and linear range of the instrument are relatively high. Determine the range of the standard curve according to the approximate concentration range of each fat-soluble vitamin in infant formula milk powder.

[0131] Experiments show that vitamin A has a good linear relationship in the concentration range of 0.5μg / mL-10μg / mL, and the curve R 2 = 0.9987; Vitamin D 2 In the concentration range of 0.002μg / mL-0.40μg / mL, the linear relationship is good, the curve R 2 = 0.9969; Vitamin D 3 In the concentration range of 0.002μg / mL-0.40μg / mL, the linear relationship is good, the curve R 2 = 0.9991; Vitamin K 1 In the concentration range of 0.05μg / mL-1.0μg / mL, the linear relationship is good, the curve R 2 =0.9966; vitamin E in the conc...

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Abstract

The invention discloses a method and a sample pretreatment method for detecting a content of fat-soluble vitamins in formula milk powder. The invention firstly discloses the sample pretreatment methodfor detecting the content of the fat-soluble vitamins in the formula milk powder, and the method comprises the following steps of weighing a to-be-detected formula milk powder sample, and adding ascorbic acid, absolute ethyl alcohol and a KOH solution for saponification; adding n-hexane into the solution after saponification, centrifuging after liquid-liquid extraction, and collecting supernatantliquid; and drying the supernatant liquid, re-dissolving and filtering to obtain a to-be-detected solution. The invention also further discloses the method for detecting the content of the fat-soluble vitamins after sample pretreatment through an ultra-high performance liquid chromatography-triple quadrupole mass spectrometry technology. The method disclosed by the invention is easy, rapid, sensitive and accurate, and can meet the detection requirements for the fat-soluble vitamins in the formula milk powder.

Description

technical field [0001] The invention relates to the field of food detection. More specifically, it relates to a method for detecting the content of fat-soluble vitamins in formula milk powder and a sample pretreatment method thereof. Background technique [0002] Vitamins are a class of nutrients necessary for the body to maintain its normal life, and they are also ingredients that must be added to infant formula milk powder. There are many types of vitamins with different chemical structures. They are usually divided into fat-soluble and water-soluble according to their solubility. The fat-soluble vitamins added to infant formula mainly include vitamins A, D, E, and K. Countries around the world have strict regulations on the types and contents of vitamins added to infant formula powder. However, from time to time, the true content of vitamins in infant formula does not match the actual label value. Since insufficient or excessive intake of vitamins can lead to dysfuncti...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/045G01N2030/062
Inventor 严华崔凤云别玮梁娜娜冯鑫张朝晖
Owner BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECH CENT
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