Study of chemical and fatty-acid compositions of phospholipids obtained from local vegetable oils and their miscella

Table 1.
Chemical shift values ​​of phospholipid compounds

№	Compound or group	con. char.	Chemical shift δ, ppm
1	CH3	а	9,00 – 9,12
2	CH2	b	8,70 – 8,74
3	–CH2CH=	d	7,95 – 8,08
4	–CH2CO–	e	7,66 – 7,74
5	–CH=CH–	c	4,60 – 4,63
6	CH2NH2	i	6,70 – 6,85
7	–CH2N^+(CH3)3	-	6,0 – 6,18
8	–N^+(CH3)3	-	6,54 – 6,77
9	–CH2OCO–	g	5,87 – 5,99
10	–CH2OPO–	h	5,64 – 5,85
11	–CHOCO–	f	4,78 – 4,80
12	–^+NH3	j	1,50 – 1,65

Below is a list of proton resonance signals, which can be used to identify the main groups of phospholipids (Table 1) [11,8].

We have recorded NMR (PMR) spectra of phospholipids obtained from various types of vegetable oils (Fig. 6).
Usually, in the PMR spectra, proton signal broadening is not detected.
According to the literature [11,8]. at 1.35 ppm - refer to proton groups. 7.5-field weak, Sp hybrid aromatic hydrocarbons come in. In the PMR spectrum, the signals in samples b) and c) are identical to sample a).
The 2-bond proton signal will last 5.5 lobes.



a) NMR (PMR) - spectroscopy of phospholipids obtained from
defatted powder (purified with acetone) hydrated with 4% distilled water of forepress cottonseed oil (Proton spectrum, spectra C13 and C13-apt additionally obtained)

b) NMR (PMR) - spectroscopy of phospholipids obtained by hydration of defatted powder (purified with acetone), forepress oil with 3% alkali NaOH (proton spectrum) (additionally obtained spectra C13 and C13-apt)

c) NMR (PMR) - spectroscopy of phospholipids obtained from defatted powder (purified with acetone), hydrated with 0.3% acetic acid of forepress cottonseed oil (Proton spectrum, additionally obtained spectra C13 and C13-apt)
Figure: 6. NMR spectra of phospholipids

Fig. 6 shows that phospholipids obtained from local vegetable oils contain almost all the main groups of surfactants.

The mass spectrum of phospholipids consists of characteristic peaks corresponding to molecular fragments with different ratios of mass to electron charge (w / e), formed as a result of bombardment of a substance with electrons in an ionization chamber and/or as a result of "cracking" during the evaporation of a substance [11,8].
The sample preparation technique depends on how it is introduced into the mass spectrometer. There are currently 3 ways to introduce the sample:
а) using a flow divider installed at the outlet of the gas-liquid chromatography, which directs part of the flow of the carrier gas with the substance directly to the mass spectrometer [8].
This method is applicable only when working with instruments that combine a mass spectrometer and gas-liquid chromatography. In this case, the sample, as soon as it is eluted from the column of the chromatograph, is automatically introduced into the spectrometer;
b) direct introduction into the spectrometer: a few millilitres (3-5) of a concentrated 15-20% solution of the sample in a volatile inert solvent such as hexane, diethyl ether (free of peroxides) or benzene is introduced with a micropipette into a glass tube with an inner diameter of 2 mm or into a capillary and evaporated to near dryness in a stream of nitrogen. The sample is placed in an ampoule, which is introduced into the vacuum system of the mass spectrometer. The system is evacuated to remove traces of solvent. The ampoule is introduced through a vacuum lock into the ion source. This technique is used when working with substances with relatively low volatility; sample weight should be 0.1-0.2 mg [12];



a) Obtained fragments of gossypol in phospholipids obtained by the traditional method of hydration of forepress cottonseed oil

b) Obtained fragments of gossypol in the conventional sense of hydrated phospholipids of extraction cottonseed oil