Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (12): 1128-1135.DOI: 10.3724/SP.J.1123.2022.01020
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MU Yingqi1,2, WU Yixuan2,3, WANG Xiao2,3, HU Liming1,*(), KE Runhui2,3,*()
Received:
2022-01-21
Online:
2022-12-08
Published:
2022-11-29
Contact:
HU Liming, KE Runhui
Supported by:
CLC Number:
MU Yingqi, WU Yixuan, WANG Xiao, HU Liming, KE Runhui. Determination of 10 organic acids in alcoholic products by ion chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2022, 40(12): 1128-1135.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2022.01020
No. | Compound | Retention time/min | Parent ion (m/z) | Product ion (m/z) | Cone voltage/V | Collision energy/eV |
---|---|---|---|---|---|---|
1 | quinic acid | 11.56 | 191.1 | 85.1* | 38 | 21 |
59.1 | 23 | |||||
2 | lactic acid | 13.94 | 89.1 | 45.1* | 22 | 11 |
43.1 | 10 | |||||
3 | succinic acid | 23.95 | 117.1 | 73.0* | 19 | 12 |
99.1 | 11 | |||||
4 | malic acid | 23.97 | 133.1 | 115.0* | 19 | 12 |
71.0 | 16 | |||||
5 | tartaric acid | 24.35 | 149.0 | 87.0* | 20 | 12 |
73.0 | 16 | |||||
6 | maleic acid | 24.85 | 115.1 | 71.1* | 15 | 15 |
27.1 | 10 | |||||
7 | fumaric acid | 25.94 | 115.1 | 71.0* | 17 | 9 |
27.0 | 11 | |||||
8 | oxalic acid | 26.17 | 89.1 | 43.0* | 20 | 12 |
45.1 | 11 | |||||
9 | citric acid | 28.36 | 191.0 | 87.0* | 18 | 12 |
111.0 | 20 | |||||
10 | aconitic acid | 30.75 | 173.0 | 85.1* | 12 | 7 |
129.1 | 11 |
Table 1 Retention times and MS parameters of the 10 organic acids
No. | Compound | Retention time/min | Parent ion (m/z) | Product ion (m/z) | Cone voltage/V | Collision energy/eV |
---|---|---|---|---|---|---|
1 | quinic acid | 11.56 | 191.1 | 85.1* | 38 | 21 |
59.1 | 23 | |||||
2 | lactic acid | 13.94 | 89.1 | 45.1* | 22 | 11 |
43.1 | 10 | |||||
3 | succinic acid | 23.95 | 117.1 | 73.0* | 19 | 12 |
99.1 | 11 | |||||
4 | malic acid | 23.97 | 133.1 | 115.0* | 19 | 12 |
71.0 | 16 | |||||
5 | tartaric acid | 24.35 | 149.0 | 87.0* | 20 | 12 |
73.0 | 16 | |||||
6 | maleic acid | 24.85 | 115.1 | 71.1* | 15 | 15 |
27.1 | 10 | |||||
7 | fumaric acid | 25.94 | 115.1 | 71.0* | 17 | 9 |
27.0 | 11 | |||||
8 | oxalic acid | 26.17 | 89.1 | 43.0* | 20 | 12 |
45.1 | 11 | |||||
9 | citric acid | 28.36 | 191.0 | 87.0* | 18 | 12 |
111.0 | 20 | |||||
10 | aconitic acid | 30.75 | 173.0 | 85.1* | 12 | 7 |
129.1 | 11 |
Fig. 3 Total ion chromatograms of the 10 organic acids with different gradient elutions a. 0-15.0 min, 0.8 mmol/L KOH; 15.0-25.0 min, 0.8-30.0 mmol/L KOH; 25.0-30.0 min, 30.0-50.0 mmol/L KOH; 30.0-35.0 min, 50.0 mmol/L KOH; 35.0-35.1 min, 50.0-0.8 mmol/L KOH; 35.1-38.0 min, 0.8 mmol/L KOH. b. 0-15.0 min, 0.8 mmol/L KOH; 15.0-25.0 min, 0.8-40.0 mmol/L KOH; 25.0-30.0 min, 40.0-60.0 mmol/L KOH; 30.0-35.0 min, 60.0 mmol/L KOH; 35.0-35.1 min, 60.0-0.8 mmol/L KOH; 35.1-38.0 min, 0.8 mmol/L KOH. c. 0-15.0 min, 0.8 mmol/L KOH; 15.0-25.0 min, 0.8-50.0 mmol/L KOH; 25.0-30.0 min, 50.0-70.0 mmol/L KOH; 30.0-35.0 min, 70.0 mmol/L KOH; 35.0-35.1 min, 70.0-0.8 mmol/L KOH; 35.1-38.0 min, 0.8 mmol/L KOH.
No. | Compound | Linear range/(mg/L) | Linear equation | r2 | LOD/(μg/L) | LOQ/(μg/L) |
---|---|---|---|---|---|---|
1 | quinic acid | 0.05-2 | Y=3.71×105X+1.97×104 | 0.9939 | 4.0 | 12.5 |
2 | lactic acid | 0.05-10 | Y=3.30×104X+3.08×103 | 0.9955 | 8.0 | 26.5 |
3 | succinic acid | 0.05-5 | Y=2.70×105X+5.52×104 | 0.9957 | 1.5 | 5.0 |
4 | malic acid | 0.05-2 | Y=4.49×105X+3.16×104 | 0.9925 | 1.5 | 5.0 |
5 | tartaric acid | 0.05-2 | Y=2.56×105X+1.22×104 | 0.9964 | 1.0 | 3.5 |
6 | maleic acid | 0.05-2 | Y=6.56×105X+1.00×104 | 0.9960 | 1.5 | 5.0 |
7 | fumaric acid | 0.05-2 | Y=2.75×105X+1.72×104 | 0.9930 | 3.5 | 12.0 |
8 | oxalic acid | 0.05-2 | Y=2.28×104X+3.78×103 | 0.9942 | 3.5 | 12.0 |
9 | citric acid | 0.05-2 | Y=2.53×105X+9.34×103 | 0.9988 | 3.0 | 10.0 |
10 | aconitic acid | 0.05-2 | Y=4.15×105X+1.29×104 | 0.9951 | 4.0 | 13.5 |
Table 2 Linear ranges, linear equations, correlation coefficients (r2), LODs, and LOQs of the 10 organic acids
No. | Compound | Linear range/(mg/L) | Linear equation | r2 | LOD/(μg/L) | LOQ/(μg/L) |
---|---|---|---|---|---|---|
1 | quinic acid | 0.05-2 | Y=3.71×105X+1.97×104 | 0.9939 | 4.0 | 12.5 |
2 | lactic acid | 0.05-10 | Y=3.30×104X+3.08×103 | 0.9955 | 8.0 | 26.5 |
3 | succinic acid | 0.05-5 | Y=2.70×105X+5.52×104 | 0.9957 | 1.5 | 5.0 |
4 | malic acid | 0.05-2 | Y=4.49×105X+3.16×104 | 0.9925 | 1.5 | 5.0 |
5 | tartaric acid | 0.05-2 | Y=2.56×105X+1.22×104 | 0.9964 | 1.0 | 3.5 |
6 | maleic acid | 0.05-2 | Y=6.56×105X+1.00×104 | 0.9960 | 1.5 | 5.0 |
7 | fumaric acid | 0.05-2 | Y=2.75×105X+1.72×104 | 0.9930 | 3.5 | 12.0 |
8 | oxalic acid | 0.05-2 | Y=2.28×104X+3.78×103 | 0.9942 | 3.5 | 12.0 |
9 | citric acid | 0.05-2 | Y=2.53×105X+9.34×103 | 0.9988 | 3.0 | 10.0 |
10 | aconitic acid | 0.05-2 | Y=4.15×105X+1.29×104 | 0.9951 | 4.0 | 13.5 |
Compound | Liquor | Yellow rice wine | Dry red wine | ||||||
---|---|---|---|---|---|---|---|---|---|
Spiked/(mg/L) | Recovery/% | RSD/% | Spiked/(mg/L) | Recovery/% | RSD/% | Spiked/(mg/L) | Recovery/% | RSD/% | |
Quinic acid | 0.1 | 96.0 | 5.6 | 0.1 | 95.7 | 5.8 | 0.1 | 108.8 | 5.8 |
0.2 | 102.0 | 2.3 | 0.2 | 99.2 | 1.9 | 0.2 | 95.5 | 6.4 | |
0.5 | 105.4 | 3.3 | 0.5 | 101.4 | 2.7 | 0.5 | 102.4 | 3.1 | |
Lactic acid | 1 | 110.2 | 3.7 | 1.0 | 99.8 | 5.9 | 1.0 | 103.9 | 1.8 |
2 | 98.9 | 4.1 | 2.0 | 105.2 | 1.6 | 2.0 | 102.4 | 2.3 | |
4 | 99.3 | 2.9 | 4.0 | 101.8 | 4.9 | 4.0 | 105.8 | 5.6 | |
Succinic acid | 0.1 | 103.1 | 3.5 | 0.1 | 104.6 | 1.3 | 0.1 | 98.7 | 2.6 |
0.2 | 107.0 | 4.3 | 0.2 | 89.5 | 2.3 | 0.2 | 96.5 | 0.5 | |
0.5 | 108.4 | 5.4 | 0.5 | 96.4 | 6.7 | 0.5 | 95.0 | 2.3 | |
Malic acid | 0.1 | 112.0 | 4.8 | 0.1 | 100.5 | 4.4 | 0.1 | 88.2 | 5.4 |
0.2 | 105.0 | 3.7 | 0.2 | 97.8 | 4.9 | 0.2 | 87.0 | 6.2 | |
0.5 | 107.8 | 4.2 | 0.5 | 103.7 | 5.8 | 0.5 | 106.2 | 2.8 | |
Tartaric acid | 0.1 | 94.0 | 6.3 | 0.1 | 102.3 | 7.2 | 0.1 | 93.2 | 1.8 |
0.2 | 101.0 | 6.0 | 0.2 | 97.8 | 5.5 | 0.2 | 84.1 | 8.9 | |
0.5 | 96.2 | 5.8 | 0.5 | 101.1 | 4.9 | 0.5 | 101.6 | 3.7 | |
Maleic acid | 0.1 | 84.4 | 3.1 | 0.1 | 104.2 | 1.3 | 0.1 | 98.3 | 3.7 |
0.2 | 105.3 | 6.8 | 0.2 | 99.7 | 6.3 | 0.2 | 102.4 | 4.1 | |
0.5 | 98.8 | 5.1 | 0.5 | 107.2 | 4.7 | 0.5 | 89.2 | 4.9 | |
Fumaric acid | 0.1 | 105.0 | 3.4 | 0.1 | 99.0 | 3.3 | 0.1 | 105.3 | 1.6 |
0.2 | 111.5 | 2.4 | 0.2 | 107.2 | 3.7 | 0.2 | 93.0 | 2.1 | |
0.5 | 100.6 | 2.6 | 0.5 | 101.3 | 8.5 | 0.5 | 111.6 | 4.1 | |
Oxalic acid | 0.1 | 101.1 | 3.7 | 0.1 | 101.0 | 4.7 | 0.1 | 107.0 | 2.1 |
0.2 | 96.5 | 5.6 | 0.2 | 103.5 | 6.2 | 0.2 | 107.5 | 3.6 | |
0.5 | 102.4 | 8.0 | 0.5 | 98.4 | 5.8 | 0.5 | 98.0 | 2.1 | |
Citric acid | 0.1 | 88.2 | 7.4 | 0.1 | 90.3 | 3.9 | 0.1 | 106.8 | 5.1 |
0.2 | 97.5 | 4.7 | 0.2 | 93.6 | 4.2 | 0.2 | 90.5 | 4.5 | |
0.5 | 101.2 | 6.2 | 0.5 | 100.7 | 3.8 | 0.5 | 83.0 | 6.8 | |
Aconitic acid | 0.1 | 94.2 | 5.8 | 0.1 | 103.0 | 4.3 | 0.1 | 112.1 | 9.0 |
0.2 | 108.5 | 3.6 | 0.2 | 90.5 | 5.6 | 0.2 | 91.2 | 9.1 | |
0.5 | 91.2 | 5.9 | 0.5 | 92.8 | 4.4 | 0.5 | 104.1 | 7.2 |
Table 3 Recoveries and relative standard deviations (RSDs) of the 10 organic acids at different spiked levels (n=6)
Compound | Liquor | Yellow rice wine | Dry red wine | ||||||
---|---|---|---|---|---|---|---|---|---|
Spiked/(mg/L) | Recovery/% | RSD/% | Spiked/(mg/L) | Recovery/% | RSD/% | Spiked/(mg/L) | Recovery/% | RSD/% | |
Quinic acid | 0.1 | 96.0 | 5.6 | 0.1 | 95.7 | 5.8 | 0.1 | 108.8 | 5.8 |
0.2 | 102.0 | 2.3 | 0.2 | 99.2 | 1.9 | 0.2 | 95.5 | 6.4 | |
0.5 | 105.4 | 3.3 | 0.5 | 101.4 | 2.7 | 0.5 | 102.4 | 3.1 | |
Lactic acid | 1 | 110.2 | 3.7 | 1.0 | 99.8 | 5.9 | 1.0 | 103.9 | 1.8 |
2 | 98.9 | 4.1 | 2.0 | 105.2 | 1.6 | 2.0 | 102.4 | 2.3 | |
4 | 99.3 | 2.9 | 4.0 | 101.8 | 4.9 | 4.0 | 105.8 | 5.6 | |
Succinic acid | 0.1 | 103.1 | 3.5 | 0.1 | 104.6 | 1.3 | 0.1 | 98.7 | 2.6 |
0.2 | 107.0 | 4.3 | 0.2 | 89.5 | 2.3 | 0.2 | 96.5 | 0.5 | |
0.5 | 108.4 | 5.4 | 0.5 | 96.4 | 6.7 | 0.5 | 95.0 | 2.3 | |
Malic acid | 0.1 | 112.0 | 4.8 | 0.1 | 100.5 | 4.4 | 0.1 | 88.2 | 5.4 |
0.2 | 105.0 | 3.7 | 0.2 | 97.8 | 4.9 | 0.2 | 87.0 | 6.2 | |
0.5 | 107.8 | 4.2 | 0.5 | 103.7 | 5.8 | 0.5 | 106.2 | 2.8 | |
Tartaric acid | 0.1 | 94.0 | 6.3 | 0.1 | 102.3 | 7.2 | 0.1 | 93.2 | 1.8 |
0.2 | 101.0 | 6.0 | 0.2 | 97.8 | 5.5 | 0.2 | 84.1 | 8.9 | |
0.5 | 96.2 | 5.8 | 0.5 | 101.1 | 4.9 | 0.5 | 101.6 | 3.7 | |
Maleic acid | 0.1 | 84.4 | 3.1 | 0.1 | 104.2 | 1.3 | 0.1 | 98.3 | 3.7 |
0.2 | 105.3 | 6.8 | 0.2 | 99.7 | 6.3 | 0.2 | 102.4 | 4.1 | |
0.5 | 98.8 | 5.1 | 0.5 | 107.2 | 4.7 | 0.5 | 89.2 | 4.9 | |
Fumaric acid | 0.1 | 105.0 | 3.4 | 0.1 | 99.0 | 3.3 | 0.1 | 105.3 | 1.6 |
0.2 | 111.5 | 2.4 | 0.2 | 107.2 | 3.7 | 0.2 | 93.0 | 2.1 | |
0.5 | 100.6 | 2.6 | 0.5 | 101.3 | 8.5 | 0.5 | 111.6 | 4.1 | |
Oxalic acid | 0.1 | 101.1 | 3.7 | 0.1 | 101.0 | 4.7 | 0.1 | 107.0 | 2.1 |
0.2 | 96.5 | 5.6 | 0.2 | 103.5 | 6.2 | 0.2 | 107.5 | 3.6 | |
0.5 | 102.4 | 8.0 | 0.5 | 98.4 | 5.8 | 0.5 | 98.0 | 2.1 | |
Citric acid | 0.1 | 88.2 | 7.4 | 0.1 | 90.3 | 3.9 | 0.1 | 106.8 | 5.1 |
0.2 | 97.5 | 4.7 | 0.2 | 93.6 | 4.2 | 0.2 | 90.5 | 4.5 | |
0.5 | 101.2 | 6.2 | 0.5 | 100.7 | 3.8 | 0.5 | 83.0 | 6.8 | |
Aconitic acid | 0.1 | 94.2 | 5.8 | 0.1 | 103.0 | 4.3 | 0.1 | 112.1 | 9.0 |
0.2 | 108.5 | 3.6 | 0.2 | 90.5 | 5.6 | 0.2 | 91.2 | 9.1 | |
0.5 | 91.2 | 5.9 | 0.5 | 92.8 | 4.4 | 0.5 | 104.1 | 7.2 |
Compound | Mild-flavor Chinese spirits | Strong-flavor Chinese spirits | Jiang-flavor Chinese spirits | Yellow rice wine | Dry red wine | ||||||
---|---|---|---|---|---|---|---|---|---|---|---|
Quinic acid | ND | ND | ND | 28.35± | 0.65 | 13.43± | 0.90 | ||||
Lactic acid | 253.82± | 1.76 | 563.13± | 10.55 | 918.34± | 5.44 | 2092.4± | 39.85 | 1569.13± | 48.49 | |
Succinic acid | 0.74± | 0.08 | 0.66± | 0.04 | 2.58± | 0.13 | 978.42± | 12.92 | 375.13± | 2.50 | |
Malic acid | ND | 0.05± | 0.01 | 0.29± | 0.02 | 36.85± | 0.94 | 248.26± | 8.43 | ||
Tartaric acid | ND | 0.06± | 0.01 | 0.09± | 0.01 | 43.93± | 0.78 | 822.24± | 11.34 | ||
Maleic acid | 0.06± | 0.01 | 0.44± | 0.04 | 1.70± | 0.03 | 44.33± | 1.57 | 7.90± | 0.13 | |
Fumaric acid | ND | ND | 0.45± | 0.03 | ND | N | D | ||||
Oxalic acid | ND | ND | ND | 4.55± | 0.13 | 31.80± | 3.67 | ||||
Citric acid | 0.06± | 0.01 | 0.03± | 0.01 | 0.05± | 0.01 | 41.23± | 1.49 | 193.10± | 4.24 | |
Aconitic acid | ND | ND | ND | ND | N | D |
Table 4 Contents of the 10 organic acids in the wine samples (n=3) mg/L
Compound | Mild-flavor Chinese spirits | Strong-flavor Chinese spirits | Jiang-flavor Chinese spirits | Yellow rice wine | Dry red wine | ||||||
---|---|---|---|---|---|---|---|---|---|---|---|
Quinic acid | ND | ND | ND | 28.35± | 0.65 | 13.43± | 0.90 | ||||
Lactic acid | 253.82± | 1.76 | 563.13± | 10.55 | 918.34± | 5.44 | 2092.4± | 39.85 | 1569.13± | 48.49 | |
Succinic acid | 0.74± | 0.08 | 0.66± | 0.04 | 2.58± | 0.13 | 978.42± | 12.92 | 375.13± | 2.50 | |
Malic acid | ND | 0.05± | 0.01 | 0.29± | 0.02 | 36.85± | 0.94 | 248.26± | 8.43 | ||
Tartaric acid | ND | 0.06± | 0.01 | 0.09± | 0.01 | 43.93± | 0.78 | 822.24± | 11.34 | ||
Maleic acid | 0.06± | 0.01 | 0.44± | 0.04 | 1.70± | 0.03 | 44.33± | 1.57 | 7.90± | 0.13 | |
Fumaric acid | ND | ND | 0.45± | 0.03 | ND | N | D | ||||
Oxalic acid | ND | ND | ND | 4.55± | 0.13 | 31.80± | 3.67 | ||||
Citric acid | 0.06± | 0.01 | 0.03± | 0.01 | 0.05± | 0.01 | 41.23± | 1.49 | 193.10± | 4.24 | |
Aconitic acid | ND | ND | ND | ND | N | D |
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