Chinese Journal of Chromatography ›› 2021, Vol. 39 ›› Issue (5): 526-533.DOI: 10.3724/SP.J.1123.2020.04028
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CHEN Shudong1,2,*(), FENG Rui1, LIN Xiaojia3, LIANG Tujin1, HE Qiuting2
Received:
2020-06-28
Online:
2021-05-08
Published:
2021-03-31
Contact:
CHEN Shudong
CLC Number:
CHEN Shudong, FENG Rui, LIN Xiaojia, LIANG Tujin, HE Qiuting. Determination of nine ginsenosides in health foods by solid extraction phase-ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2021, 39(5): 526-533.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2020.04028
No. | Com- pound | tR/ min | Q1/Q3 ion pairs (m/z) | Collision energy/ eV | Tube lens/ V |
---|---|---|---|---|---|
1 | Rg1 | 8.01 | 799.5/637.5*, 799.5/475.5 | 26, 33 | 150 |
2 | Re | 8.19 | 945.5/637.4*, 945.5/475.5 | 51, 36 | 180 |
3 | Rf | 11.82 | 799.5/475.4*, 799.5/637.4 | 36, 30 | 150 |
4 | Rg2 | 13.86 | 783.5/475.4*, 783.5/637.4 | 36, 26 | 150 |
5 | Rb1 | 15.13 | 1153.6/1107.7*, 1153.6/221.1 | 28, 56 | 180 |
6 | Rc | 16.32 | 1077.6/783.5*, 1077.6/945.5 | 41, 40 | 180 |
7 | Rb2 | 17.42 | 1077.6/783.5*, 1077.6/945.5 | 46, 38 | 175 |
8 | Rb3 | 17.69 | 1077.6/783.5*, 1077.6/945.5 | 42, 41 | 180 |
9 | Rd | 18.63 | 945.5/783.5*, 945.5/621.4 | 36, 40 | 164 |
Table 1 MS/MS parameters of the nine analytes
No. | Com- pound | tR/ min | Q1/Q3 ion pairs (m/z) | Collision energy/ eV | Tube lens/ V |
---|---|---|---|---|---|
1 | Rg1 | 8.01 | 799.5/637.5*, 799.5/475.5 | 26, 33 | 150 |
2 | Re | 8.19 | 945.5/637.4*, 945.5/475.5 | 51, 36 | 180 |
3 | Rf | 11.82 | 799.5/475.4*, 799.5/637.4 | 36, 30 | 150 |
4 | Rg2 | 13.86 | 783.5/475.4*, 783.5/637.4 | 36, 26 | 150 |
5 | Rb1 | 15.13 | 1153.6/1107.7*, 1153.6/221.1 | 28, 56 | 180 |
6 | Rc | 16.32 | 1077.6/783.5*, 1077.6/945.5 | 41, 40 | 180 |
7 | Rb2 | 17.42 | 1077.6/783.5*, 1077.6/945.5 | 46, 38 | 175 |
8 | Rb3 | 17.69 | 1077.6/783.5*, 1077.6/945.5 | 42, 41 | 180 |
9 | Rd | 18.63 | 945.5/783.5*, 945.5/621.4 | 36, 40 | 164 |
Fig. 1 Chemical structures of the nine ginsenosides Arap: α-L-arabinopyranosyl; Araf: α-L-arabinofuranosyl; Glc: β-D-glucose; Xyl: β-D-xylopyranosyl; Rha: α-L-rhamnopyranosyl.
Compound | MEs/% | Recoveries/% | ||||||
---|---|---|---|---|---|---|---|---|
C18 | HLB | Alumina-N/XAD-2 | C18 | HLB | Alumina-N/XAD-2 | |||
Rg1 | 55.2 | 68.1 | 91.5 | 65.6 | 88.2 | 101.4 | ||
Re | 48.6 | 72.2 | 93.3 | 68.9 | 79.3 | 107.6 | ||
Rf | 51.5 | 70.3 | 89.6 | 75.5 | 95.6 | 96.7 | ||
Rg2 | 62.3 | 89.1 | 94.4 | 69.4 | 117.9 | 93.5 | ||
Rb1 | 46.5 | 82.6 | 95.3 | 72.5 | 124.8 | 89.7 | ||
Rc | 54.2 | 74.1 | 89.9 | 70.4 | 94.2 | 90.6 | ||
Rb2 | 55.3 | 63.3 | 90.1 | 78.6 | 90.4 | 98.4 | ||
Rb3 | 63.9 | 79.4 | 91.7 | 59.4 | 80.1 | 103.4 | ||
Rd | 57.6 | 66.5 | 92.3 | 69.1 | 78.5 | 94.5 |
Table 2 MEs and recoveries of the nine ginsenosides using different SPE columns
Compound | MEs/% | Recoveries/% | ||||||
---|---|---|---|---|---|---|---|---|
C18 | HLB | Alumina-N/XAD-2 | C18 | HLB | Alumina-N/XAD-2 | |||
Rg1 | 55.2 | 68.1 | 91.5 | 65.6 | 88.2 | 101.4 | ||
Re | 48.6 | 72.2 | 93.3 | 68.9 | 79.3 | 107.6 | ||
Rf | 51.5 | 70.3 | 89.6 | 75.5 | 95.6 | 96.7 | ||
Rg2 | 62.3 | 89.1 | 94.4 | 69.4 | 117.9 | 93.5 | ||
Rb1 | 46.5 | 82.6 | 95.3 | 72.5 | 124.8 | 89.7 | ||
Rc | 54.2 | 74.1 | 89.9 | 70.4 | 94.2 | 90.6 | ||
Rb2 | 55.3 | 63.3 | 90.1 | 78.6 | 90.4 | 98.4 | ||
Rb3 | 63.9 | 79.4 | 91.7 | 59.4 | 80.1 | 103.4 | ||
Rd | 57.6 | 66.5 | 92.3 | 69.1 | 78.5 | 94.5 |
Compound | Linear equation | r2 | 10 mg/kg | 60 mg/kg | 120 mg/kg | ||||||
---|---|---|---|---|---|---|---|---|---|---|---|
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||||
Rg1 | Y=6.68×106X+4.49×105 | 0.9994 | 97.1 | 1.0 | 102.5 | 3.5 | 111.8 | 1.5 | |||
Re | Y=1.66×107X+2.17×106 | 0.9970 | 108.6 | 8.0 | 97.2 | 1.2 | 110.3 | 0.8 | |||
Rf | Y=5.14×106X+6.44×106 | 0.9963 | 114.2 | 1.8 | 97.5 | 2.3 | 106.2 | 0.8 | |||
Rg2 | Y=4.21×106X+3.09×106 | 0.9991 | 109.8 | 4.7 | 91.6 | 0.9 | 97.2 | 1.8 | |||
Rb1 | Y=1.39×106X+1.82×106 | 0.9969 | 81.4 | 5.7 | 85.1 | 3.3 | 89.1 | 4.4 | |||
Rc | Y=2.16×106X+1.61×106 | 0.9989 | 104.5 | 3.6 | 92.5 | 0.4 | 96.6 | 1.8 | |||
Rb2 | Y=1.98×106X+1.90×106 | 0.9983 | 106.7 | 3.0 | 93.7 | 3.6 | 100.7 | 0.6 | |||
Rb3 | Y=1.94×106X+1.93×106 | 0.9984 | 102.7 | 4.8 | 95.7 | 3.0 | 101.8 | 0.5 | |||
Rd | Y=1.87×106X+2.51×106 | 0.9965 | 108.3 | 1.9 | 92.3 | 3.7 | 103.5 | 2.3 |
Table 3 Linear equations, correlation coefficients (r2), spiked recoveries and RSDs of the nine ginsenosides (n=6)
Compound | Linear equation | r2 | 10 mg/kg | 60 mg/kg | 120 mg/kg | ||||||
---|---|---|---|---|---|---|---|---|---|---|---|
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||||
Rg1 | Y=6.68×106X+4.49×105 | 0.9994 | 97.1 | 1.0 | 102.5 | 3.5 | 111.8 | 1.5 | |||
Re | Y=1.66×107X+2.17×106 | 0.9970 | 108.6 | 8.0 | 97.2 | 1.2 | 110.3 | 0.8 | |||
Rf | Y=5.14×106X+6.44×106 | 0.9963 | 114.2 | 1.8 | 97.5 | 2.3 | 106.2 | 0.8 | |||
Rg2 | Y=4.21×106X+3.09×106 | 0.9991 | 109.8 | 4.7 | 91.6 | 0.9 | 97.2 | 1.8 | |||
Rb1 | Y=1.39×106X+1.82×106 | 0.9969 | 81.4 | 5.7 | 85.1 | 3.3 | 89.1 | 4.4 | |||
Rc | Y=2.16×106X+1.61×106 | 0.9989 | 104.5 | 3.6 | 92.5 | 0.4 | 96.6 | 1.8 | |||
Rb2 | Y=1.98×106X+1.90×106 | 0.9983 | 106.7 | 3.0 | 93.7 | 3.6 | 100.7 | 0.6 | |||
Rb3 | Y=1.94×106X+1.93×106 | 0.9984 | 102.7 | 4.8 | 95.7 | 3.0 | 101.8 | 0.5 | |||
Rd | Y=1.87×106X+2.51×106 | 0.9965 | 108.3 | 1.9 | 92.3 | 3.7 | 103.5 | 2.3 |
Sample | Rg1 | Re | Rf | Rg2 | Rb1 | Rc | Rb2 | Rb3 | Rd | Total |
---|---|---|---|---|---|---|---|---|---|---|
1 | 0.0874 | 0.202 | ND | 0.0358 | 0.0162 | 0.0529 | 0.129 | 0.275 | 0.197 | 1.00 |
2 | 0.0700 | 0.214 | <0.0010 | 0.00144 | 0.175 | 0.0460 | 0.00977 | 0.0112 | 0.104 | 0.63 |
3 | 0.229 | 0.0184 | <0.0010 | 0.00341 | 0.0671 | <0.0010 | ND | <0.0010 | 0.0424 | 0.56 |
4 | 0.417 | 0.0549 | <0.0010 | 0.0178 | 0.149 | <0.0010 | <0.0010 | <0.0010 | 0.0985 | 0.74 |
5 | 0.0746 | 0.245 | ND | 0.0336 | 0.233 | 0.0914 | 0.0206 | 0.0280 | 0.126 | 0.85 |
6 | 0.201 | 0.510 | ND | 0.0640 | 0.0469 | 0.0950 | 0.284 | 0.770 | 0.709 | 2.68 |
7 | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
8 | 0.140 | 0.153 | 0.00114 | 0.00915 | 0.00910 | 0.0370 | 0.0376 | 0.0242 | 0.0438 | 0.46 |
9 | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
10 | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
11 | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
Table 4 Detected results of the nine ginsenosides in health food samples%
Sample | Rg1 | Re | Rf | Rg2 | Rb1 | Rc | Rb2 | Rb3 | Rd | Total |
---|---|---|---|---|---|---|---|---|---|---|
1 | 0.0874 | 0.202 | ND | 0.0358 | 0.0162 | 0.0529 | 0.129 | 0.275 | 0.197 | 1.00 |
2 | 0.0700 | 0.214 | <0.0010 | 0.00144 | 0.175 | 0.0460 | 0.00977 | 0.0112 | 0.104 | 0.63 |
3 | 0.229 | 0.0184 | <0.0010 | 0.00341 | 0.0671 | <0.0010 | ND | <0.0010 | 0.0424 | 0.56 |
4 | 0.417 | 0.0549 | <0.0010 | 0.0178 | 0.149 | <0.0010 | <0.0010 | <0.0010 | 0.0985 | 0.74 |
5 | 0.0746 | 0.245 | ND | 0.0336 | 0.233 | 0.0914 | 0.0206 | 0.0280 | 0.126 | 0.85 |
6 | 0.201 | 0.510 | ND | 0.0640 | 0.0469 | 0.0950 | 0.284 | 0.770 | 0.709 | 2.68 |
7 | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
8 | 0.140 | 0.153 | 0.00114 | 0.00915 | 0.00910 | 0.0370 | 0.0376 | 0.0242 | 0.0438 | 0.46 |
9 | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
10 | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
11 | ND | ND | ND | ND | ND | ND | ND | ND | ND | ND |
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