Determination of fatty acids compositions and contents in Chinese mitten crabs by gas chromatography

doi:10.3724/SP.J.1123.2021.01032

Abstract

Abstract:

Determination of fatty acid compositions and contents in Chinese mitten crabs is of great significance to evaluate its nutritional value and quality. However, in the face of a wide range of fatty acid extraction and methyl esterification reagents, the measurement results are uneven, and it is difficult to accurately quantify the rich fatty acids in Chinese mitten crabs. In this paper, four kinds of oil extraction reagents and two kinds of methylating reagents, were investigated. Chloroform-methanol (1∶1, v/v) was used as the extraction solvent, and methanol containing 2% sulfuric acid was used as the derivatization reagent. A method for the determination of fatty acids in the muscle of Chinese mitten crabs by gas chromatography was established. The experiment was carried out under the condition of programmed temperature rise, 37 kinds of fatty acids were separated on a DM-2560 capillary column (100 m×0.25 mm×0.20 μm), detected by hydrogen flame ionization detector (FID) and quantified by external standard method. The linear relationships of the 37 fatty acids were good in the range of 0.5-100.0 μg/mL. The correlation coefficients (R²) were 0.9981-0.9999. The limits of detection (LODs) and limits of quantification (LOQs) were 0.01-0.02 mg/100 g and 0.04-0.06 mg/100 g, respectively. The methodology was validated by palmitic acid and stearic acid. The recoveries were 76.0%-97.5%, and the relative standard deviations (RSD, n=5) were 3.31%-7.90% at the spiked levels of 1, 2 and 10 mg/100 g. The method was applied to the determination of fatty acid compositions and contents in the muscle of Chinese mitten crabs. A total of 31 kinds of fatty acids were detected. The length of carbon chain ranged from 12 to 24, and the total content of fatty acids reached 281.03 mg/100 g. Oleic acid, docosahexaenoic acid and eicosapentaenoic acid were the main fatty acids in the muscle of Chinese mitten crabs. Thus, this method provided accurate and reliable theoretical data for the determination of fatty acids in Chinese mitten crabs. This method has the advantages of simple operation, small amount of reagent and sample, reliable qualitative, accurate quantitative, detection of more fatty acid types. It is suitable for the rapid detection of fatty acid compositions and contents in muscle tissue of Chinese mitten crabs.

Key words: gas chromatography (GC), fatty acids, Chinese mitten crabs

CLC Number:

O658

SHEN Zhaodong, HUANG Dongmei, FANG Changling, YE Hongli, TIAN Liangliang, WU Zi, ZHANG Jun. Determination of fatty acids compositions and contents in Chinese mitten crabs by gas chromatography[J]. Chinese Journal of Chromatography, 2021, 39(12): 1340-1346.

Figures/Tables 9

References

[1]	Zhang Z Q, Huang D M, Cai Y Q, et al. Food Science, 2020, 41(24):125
[1]	张政权, 黄冬梅, 蔡友琼, 等. 食品科学, 2020, 41(24):125
[2]	Xie Q S, Liu Y R. Aquac Res, 2020, 51(7):2948
[3]	Lin J. Guangdong Chemical Industry, 2013, 40(6):92
[3]	林杰. 广东化工, 2013, 40(6):92
[4]	Chen Z H, Hu H Y, Chen Y, et al. Medical Guide, 2018, 37(11):1334
[4]	陈则华, 胡慧芸, 陈鹰, 等. 医药导报, 2018, 37(11):1334
[5]	Jaddoa H H, Hameed I H, Mohammed G J. Orient J Chem, 2016, 32(4):2107
[6]	Qiu R F, Huang Z P, Wang L L. Chinese Journal of Chromatography, 2018, 36(9):925
[6]	邱若风, 黄忠平, 王丽丽. 色谱, 2018, 36(9):925
[7]	Liu W Y, Jia W, Wu T, et al. Chinese Journal of Chromatography, 2016, 34(11):1113
[7]	刘文媛, 贾伟, 吴婷, 等. 色谱, 2016, 34(11):1113
[8]	Wu Y W, Li B N, Wang Y, et al. Journal of Food Safety and Quality Inspection, 2015, 6(9):37
[8]	武彦文, 李冰宁, 汪雨, 等. 食品安全质量检测学报, 2015, 6(9):37
[9]	Liu P S, Mou Y, Ma A D, et al. Journal of Instrumental Analysis, 2020, 39(8):1000
[9]	刘佩珊, 牟燕, 马安德, 等. 分析测试学报, 2020, 39(8):1000
[10]	Yan K, Liu X T, Liu Y, et al. Journal of Food Safety and Quality Inspection, 2020, 11(1):82
[10]	晏凯, 刘晓彤, 刘悦, 等. 食品安全质量检测学报, 2020, 11(1):82
[11]	Tian C X, Wang Y Y, Wu S M, et al. Physical Testing and Chemical Analysis Part B: Chemical Analysis, 2020, 56(6):66
[11]	田春霞, 王远远, 吴苏妙, 等. 理化检验(化学分册), 2020, 56(6):66
[12]	Zhuang H Q, Liu J Q, Zhong Y, et al. Modern Food Technology, 2020, 36(9):10
[12]	庄海旗, 刘江琴, 钟宇, 等. 现代食品科技, 2020, 36(9):10
[13]	Jiang X D, Wang H N, Cheng Y X, et al. Aquac, 2020, 523(1):194
[14]	Wang X, Han G, Zhang X J, et al. Journal of Dalian Ocean University, 2019, 34(5):688
[14]	王潇, 韩刚, 张小军, 等. 大连海洋大学学报, 2019, 34(5):688
[15]	Zhang D L, Chen Y, Zhou G T. China Condiment, 2007(10):30
[15]	张道雷, 陈瑶, 周广田. 中国调味品, 2007(10):30
[16]	Heymann H, Hedrick H B, Karrasch M A. J Food Sci, 2010, 55(3):613

No.	Compound	Regression equation	R²	LOD/ (mg/100 g)	LOQ/ (mg/100 g)
1	C4∶0	y=2.127x+0.385	0.9982	0.01	0.04
2	C6∶0	y=1.418x+0.043	0.9997	0.01	0.04
3	C8∶0	y=1.406x+0.062	0.9994	0.01	0.04
4	C10∶0	y=1.388x+0.145	0.9998	0.01	0.04
5	C11∶0	y=0.681x+0.146	0.9992	0.02	0.06
6	C12∶0	y=1.430x+0.127	0.9993	0.01	0.04
7	C13∶0	y=0.711x+0.131	0.9996	0.02	0.06
8	C14∶0	y=1.446x+0.172	0.9999	0.01	0.04
9	C14∶1	y=0.711x+0.134	0.9999	0.02	0.06
10	C15∶0	y=0.739x+0.086	0.9987	0.02	0.06
11	C15∶1	y=0.727x+0.118	0.9999	0.02	0.06
12	C16∶0	y=2.244x+0.251	0.9995	0.01	0.04
13	C16∶1	y=0.714x+0.102	0.9988	0.02	0.06
14	C17∶0	y=0.767x+0.066	0.9999	0.02	0.06
15	C17∶1	y=0.751x+0.097	0.9989	0.02	0.06
16	C18∶0	y=1.501x+0.143	0.9989	0.01	0.04
17	C18∶1n9t	y=0.751x+0.064	0.9983	0.02	0.06
18	C18∶1n9c	y=1.536x+0.161	0.9981	0.01	0.04
19	C18∶2n6t	y=0.746x+0.100	0.9999	0.02	0.06
20	C18∶2n6c	y=0.773x+0.101	0.9986	0.02	0.06
21	C20∶0	y=1.528x+0.152	0.9987	0.01	0.04
22	C18∶3n6	y=0.742x+0.173	0.9997	0.02	0.06
23	C20∶1	y=0.781x+0.145	0.9996	0.02	0.06
24	C18∶3n3	y=0.784x+0.139	0.9997	0.02	0.06
25	C21∶0	y=0.762x+0.136	0.9996	0.02	0.06
26	C20∶2	y=0.762x+0.130	0.9999	0.02	0.06
27	C22∶0	y=1.578x+0.171	0.9987	0.01	0.04
28	C20∶3n6	y=0.769x+0.139	0.9989	0.02	0.06
29	C22∶1n9	y=0.762x+0.158	0.9992	0.02	0.06
30	C20∶3n3	y=1.568x+0.126	0.9993	0.02	0.06
31	C20∶4n6	y=0.746x+0.113	0.9998	0.02	0.06
32	C23∶0	y=0.784x+0.104	0.9999	0.02	0.06
33	C22∶2	y=0.784x+0.101	0.9999	0.02	0.06
34	C24∶0	y=0.776x+0.158	0.9989	0.01	0.04
35	C20∶5n3	y=1.648x+0.171	0.9991	0.02	0.50
36	C24∶1	y=0.772x+0.152	0.9998	0.02	0.06
37	C22∶6n3	y=0.673x+0.126	0.9999	0.02	0.06

No.	Compound	Regression equation	R²	LOD/ (mg/100 g)	LOQ/ (mg/100 g)
1	C4∶0	y=2.127x+0.385	0.9982	0.01	0.04
2	C6∶0	y=1.418x+0.043	0.9997	0.01	0.04
3	C8∶0	y=1.406x+0.062	0.9994	0.01	0.04
4	C10∶0	y=1.388x+0.145	0.9998	0.01	0.04
5	C11∶0	y=0.681x+0.146	0.9992	0.02	0.06
6	C12∶0	y=1.430x+0.127	0.9993	0.01	0.04
7	C13∶0	y=0.711x+0.131	0.9996	0.02	0.06
8	C14∶0	y=1.446x+0.172	0.9999	0.01	0.04
9	C14∶1	y=0.711x+0.134	0.9999	0.02	0.06
10	C15∶0	y=0.739x+0.086	0.9987	0.02	0.06
11	C15∶1	y=0.727x+0.118	0.9999	0.02	0.06
12	C16∶0	y=2.244x+0.251	0.9995	0.01	0.04
13	C16∶1	y=0.714x+0.102	0.9988	0.02	0.06
14	C17∶0	y=0.767x+0.066	0.9999	0.02	0.06
15	C17∶1	y=0.751x+0.097	0.9989	0.02	0.06
16	C18∶0	y=1.501x+0.143	0.9989	0.01	0.04
17	C18∶1n9t	y=0.751x+0.064	0.9983	0.02	0.06
18	C18∶1n9c	y=1.536x+0.161	0.9981	0.01	0.04
19	C18∶2n6t	y=0.746x+0.100	0.9999	0.02	0.06
20	C18∶2n6c	y=0.773x+0.101	0.9986	0.02	0.06
21	C20∶0	y=1.528x+0.152	0.9987	0.01	0.04
22	C18∶3n6	y=0.742x+0.173	0.9997	0.02	0.06
23	C20∶1	y=0.781x+0.145	0.9996	0.02	0.06
24	C18∶3n3	y=0.784x+0.139	0.9997	0.02	0.06
25	C21∶0	y=0.762x+0.136	0.9996	0.02	0.06
26	C20∶2	y=0.762x+0.130	0.9999	0.02	0.06
27	C22∶0	y=1.578x+0.171	0.9987	0.01	0.04
28	C20∶3n6	y=0.769x+0.139	0.9989	0.02	0.06
29	C22∶1n9	y=0.762x+0.158	0.9992	0.02	0.06
30	C20∶3n3	y=1.568x+0.126	0.9993	0.02	0.06
31	C20∶4n6	y=0.746x+0.113	0.9998	0.02	0.06
32	C23∶0	y=0.784x+0.104	0.9999	0.02	0.06
33	C22∶2	y=0.784x+0.101	0.9999	0.02	0.06
34	C24∶0	y=0.776x+0.158	0.9989	0.01	0.04
35	C20∶5n3	y=1.648x+0.171	0.9991	0.02	0.50
36	C24∶1	y=0.772x+0.152	0.9998	0.02	0.06
37	C22∶6n3	y=0.673x+0.126	0.9999	0.02	0.06

Compound	Background/ (mg/100 g)	Added/ (mg/100 g)	Found/ (mg/100 g)	Recovery/ %	RSD/ %
C16∶0	16.19	1	16.95	76.0	6.80
		2	18.14	97.5	7.90
		10	25.04	88.5	3.31
C18∶0	10.02	1	10.95	93.0	5.78
		2	11.93	95.5	6.15
		10	19.03	90.1	3.55

Compound	Background/ (mg/100 g)	Added/ (mg/100 g)	Found/ (mg/100 g)	Recovery/ %	RSD/ %
C16∶0	16.19	1	16.95	76.0	6.80
		2	18.14	97.5	7.90
		10	25.04	88.5	3.31
C18∶0	10.02	1	10.95	93.0	5.78
		2	11.93	95.5	6.15
		10	19.03	90.1	3.55

Compound	Content/ (mg/100 g)	Percentage composition/%	RSD/%
C12∶0	0.12	0.04	2.70
C14∶0	1.60	0.57	3.11
C14∶1	0.53	0.19	3.96
C15∶0	1.20	0.43	2.68
C15∶1	0.09	0.03	2.08
C16∶0	16.19	5.81	4.36
C16∶1	19.92	7.07	5.85
C17∶0	5.75	2.04	3.28
C17∶1	2.65	0.94	2.76
C18∶0	10.02	3.58	4.81
C18∶1n9t	1.54	0.55	2.69
C18∶1n9c	33.29	11.83	5.90
C18∶2n6t	0.47	0.17	2.30
C18∶2n6c	23.35	8.32	5.28
C20∶0	0.67	0.24	2.36
C18∶3n6	1.76	0.60	2.11
C20∶1	6.38	2.25	3.41
C18∶3n3	6.05	2.23	3.69
C21∶0	0.88	0.31	1.96
C20∶2	4.24	1.49	2.20
C22∶0	0.44	0.15	2.11
C20∶3n6	2.33	0.82	2.69
C22∶1n9	4.37	1.55	3.69
C20∶3n3	1.25	0.45	3.40
C20∶4n6	0.13	0.05	2.96
C23∶0	10.44	3.78	3.55
C22∶2	1.05	0.37	2.69
C24∶0	0.15	0.05	2.30
C20∶5n3 EPA	55.78	19.74	2.96
C24∶1	0.84	0.31	3.11
C22∶6n3 DHA	67.57	24.02	5.36
∑SFA	47.46	17.01
∑MUFA	69.61	24.72
∑PUFA	163.96	58.27
ω-3/ω-6	4.74
Total	281.03	100.00