Determination of terpenoids in Baijiu using solid-phase extraction combined with headspace solid-phase microextraction

Figures & data

Table 1. Temperature program.

	Rate (°C/min)	Temperature (°C)	Hold Time (min)
Initial		40.0	1.00
1	4.0	200	0.00
2	20.0	250.0	10.00

Figure 1. Comparison of terpene extraction capacity of SPE extraction columns from different manufacturers.

Figure 2. Effect of different ultrapure water cleaning volume on terpene species.

Figure 3. The effect of extraction temperature on terpenes.

Figure 4. The effect of extraction time on terpenes.

Table 2. Terpenes of Laobaiganxiangxing baijiu.

Serial number	Peak time	Compound name	Peak area	CAS number
1	7.935	β-Ocimene	97318	13877–91-3
2	11.195	D-Limonene	568508	138–86-3
3	13.045	Citral	695903	5392–40-5
4	15.615	p-Cymene	368938	99–87-6
5	22.09	(+)-Cyclosativene	341637	22469–52-9
6	22.705	2,5,5-Trimethyl-2,3,4,5,6,7-hexahydro-1 H-2,4a-ethanonaphthalene	261838	32391–44-9
7	23.07	Thujopsene	165603	470–40-6
8	23.43	(+)-Calarene	93961	17334–55-3
9	23.76	(+)-Sativen	172546	3650–28-0
10	24.31	α-Bulnesene	1164115	3772–93-8
11	24.39	α-Gurjunene	3117121	489–40-7
12	24.705	Caryophyllene	2357601	87–44-5
13	24.935	Longifolene	579314	475–20-7
14	25.065	cis-Thujopsene	469840	470–40-6
15	25.395	3-Isopropyl-6,8a-dimethyl-1,2,4,5,8,8a-hexahydroazulene	184564	16661–00-0
16	25.61	6S-2,3,8,8-Tetramethyltricyclo[5.2.2.0(1,6)]undec-2-ene	129730	137235–48-4
17	26.2	α-Funebrene	72129	50894–66-1
18	26.505	(+)-Valencene	24323	4630–07-3
19	27.07	Guaia-1(10),11-diene	83383	3691–11-0
20	27.66	γ-Muurolene	58463	30021–74-0
21	27.855	Isoledene	53414	95910–36-4
22	27.935	δ-Cadinene	200208	483–76-1
23	52.865	Squalene	1542913	7683–64-9

Table 3. Regression equation, correlation coefficient and recovery of 4 components.

compound	Regression equation	R^2	LOD/ (ug/L)	LOQ/ (ug/L)	Recovery rate (%)	RSD (%)
Caryophyllene	y = 573500x + 373057	R^2 = 0.9922	0.24	0.75	71.69	4. 47
D-Limonene	y = 14498x + 24103	R^2 = 0.9945	0.49	1.66	118.31	3.34
Squalene	y = 48928x + 168907	R^2 = 0.9938	6.69	21.84	120.23	3.51
p-Cymene	y = 14914x – 68509	R^2 = 0.9901	3.52	11.74	80.72	4.21

Figure 5. The chromatograms of the terpenoids of the six Baijiu samples.

Data availability statement

Data not available due to commercial restrictions.