High Performance Liquid Chromatography Detection Protocol for Poppy Shell Alkaloids in Foods

In the past two days, Lu Chuang Instrument Xiaobian heard that the foods operated by many catering service units in the country were popped up with poppy alkaloids. The foods involved were hot pot, lo mei, snacks, grilled fish, stir-fry, etc. (all kinds are perfect, it is impossible to prevent) On January 20, the State Food and Drug Administration issued the Notice on the Detection of Poppy Shell Ingredients in Foods Operated by 35 Catering Service Units. So Lu Chuang instrument Xiaobian seriously checked the poppy shell is a cockroach, but also found a picture, this thing Xiaobian how to look a bit familiar?

The poppy shell contains a variety of alkaloids. The main components are morphine, codeine, narcotine, papaverine, and thebaine. Although the content is small, its "utility" cannot be underestimated. In the hot pot, the alkaloids in the poppy shell are mainly used as a flavoring agent for spicy flavors, which form a wrong stimulation to the pain caused by the spicy taste. After eating, the human body can be in a special state of pleasure, and thus gradually become dependent. Sex and addiction. Long-term consumption of foods containing poppy shells can also cause damage to the human nervous system and may cause chronic poisoning.

Poppy shells are listed in the “List of non-edible substances and misusable food additives that may be illegally added in foods” issued by the State in 2009, and may indicate the types of foods that may be added: hot pot, hot pot bottom, snacks, and lo mei products. Even drinks, but some unscrupulous merchants take risks in order to attract customers.

Lu Chuang analysis instrument has long been a method for the detection of poppy alkaloids. If you don't believe, please look down!

Sample processing - simple

Lu record user equipment for intensive studies to develop a method for detecting in food poppy capsule alkaloids, multiple reaction monitoring mode, effectively eliminate matrix interference, the samples were solvent extracted, using solid phase extraction column purification, high-performance liquid Chromatographic separation (HPLC) analysis can be used to determine the five alkaloids in papalin, thebaine, morphine, narcotine, and codeine.

Detection method - efficient

1. Scope of application

It is suitable for the determination of five kinds of alkaloids such as papaverine, tibain, morphine, narcotine and codeine in foods such as hot pot, hot pot bottom, snacks, lo mei products and even beverages.

2, extract

Weigh 2 g of the sample to be tested in a 50 mL stoppered plastic centrifuge tube, add 10 mL of 0.1 mol/L hydrochloric acid, mix and sonicate for 30 min, and centrifuge at 8000 r/min at 4 °C. 6 min, collect the aqueous phase into another 50 mL centrifuge tube, add 10 mL of hydrochloric acid solution to the original centrifuge tube, repeat the above operation, add the extract, add 10 mL of petroleum ether, vortex for 10 seconds, and then set the fraction. The layer (also can be layered by centrifugation), the organic phase is discarded, and purified by a solid phase extraction column.

3, purification

a. Activation: 5 mL of methanol, 5 mL of water were added in sequence, and the effluent was discarded.

b. Loading: The extract was passed through a PXC column at a rate of about 2 to 3 drops per second, and the effluent was discarded.

c. Rinse: Rinse the extraction column with 5 mL of methanol and 5 mL of water in turn, and discard the effluent.

d. Elution: 6 mL of 5% ammonia in methanol, and the eluent was collected.

e. Re-dissolution: The eluate was dried by nitrogen at 40 ° C, re-dissolved with 10% aqueous methanol, and determined by HPLC.

4, instrument conditions

Column: Agilent XDB-C18 (4.6 × 150 mm), ultraviolet detection wavelength of morphine 210 nm, codeine 213 nm, papaverine 253 nm, quantitative analysis by external standard method.

Flow rate: 0.3 mL / min

Injection volume: 5 μL

Column temperature: 40 ° C

Mobile phase: A: 0.1% aqueous formic acid, B: methanol

Test results - reliable

The linear range, precision, spiked recovery, detection limit and limit of quantitation of the method were investigated rigorously. The detection limit and limit of quantification of the method were better than the Shanghai local standard DB 31/2010-2012. Provisions for the determination of papaverine, morphine, narcotine, codeine and thebaine in hot pot food.