T/BDAS 001-2021 Active Group standards

T/BDAS 001-2021 Determination of Melatonin Content in Milk by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS)

Publish Date: 2021-08-11 Implement Date: 2021-09-10 For services related to genuine standard inquiry, procurement, translation, and other related services in China, please Contact Us

Price: $ 20.00

Out of stock

Basic Information

Standard Code: T/BDAS 001-2021

Standard Type: Group standards

Standard Status: Active

is_force_gb: no

CCS Name: Food

ICS Name: Milk and processed milk products

Publish Date: 2021-08-11

Implement Date: 2021-09-10

Scope

Scope: This document specifies the liquid chromatography-tandem mass spectrometry method for the determination of melatonin content in milk. This document is applicable to the determination of melatonin in raw milk, pasteurized milk, and sterilized milk. The detection limit of the method in this document is 0.04 μg/L, and the quantification limit is 0.10 μg/L. Main technical content: This standard specifies the liquid chromatography-tandem mass spectrometry method for the determination of melatonin content in milk, which is applicable to the determination of melatonin content in raw milk, pasteurized milk, and sterilized milk. Extraction method: Take an appropriate amount of sample and place it in an ultrasonic cleaner at 37°C for 30 minutes to fully mix the sample. Accurately transfer 1 mL of the sample to a 15 mL centrifuge tube, accurately add 4 mL of methanol, and use a vortex mixer to shake and extract for 10 minutes. Store at -18°C for 30 minutes. Use a low-temperature high-speed centrifuge at 10000 g and 4°C for 5 minutes. Filter the supernatant through a 0.22 μm organic phase filter membrane into a sample bottle to obtain the sample solution for liquid chromatography-tandem mass spectrometry determination. Technical point 1: Methanol as a solvent for melatonin not only does not affect the stability of the target substance in the sample, but also can cause protein denaturation and precipitation in milk. By mixing the sample to be tested and methanol in a 1:4 ratio and using a one-step extraction method with methanol solvent, no purification is required, reducing losses caused by the degreasing process. Technical point 2: Milk and its dairy products contain a large number of fat globules of different sizes. Ultrasound (30 minutes) can produce cavitation in the liquid and break down the fat globules in milk. Shaking and extracting with a vortex mixer for 10 minutes allows the supernatant to be centrifuged without losing melatonin. Technical point