Chinese Journal of Chromatography ›› 2021, Vol. 39 ›› Issue (5): 518-525.DOI: 10.3724/SP.J.1123.2020.06022
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LI Hui1, CUI Lanchong2, ZHANG Guolei1, ZHANG Mengmeng1, JIAO Lili1, WU Wei1,*()
Received:
2020-06-30
Online:
2021-05-08
Published:
2021-03-31
Contact:
WU Wei
Supported by:
CLC Number:
LI Hui, CUI Lanchong, ZHANG Guolei, ZHANG Mengmeng, JIAO Lili, WU Wei. Quantitative analysis of tryptophan and its metabolites in urine by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2021, 39(5): 518-525.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2020.06022
Compound | tR/min | Mr | Number of dansyl group | Precursor ion (m/z) | Product ion (m/z) | Collision energy/eV | RF lens |
---|---|---|---|---|---|---|---|
3-OH-Kyn | 3.86 | 224.08 | 2 | 691.14 | 171.14* | 37.54 | 98.31 |
456.15 | 27.48 | ||||||
349.37 | 14.98 | ||||||
3-OH-AA | 4.25 | 153.04 | 1 | 387.09 | 171.15* | 17.59 | 85.73 |
216.19 | 15.36 | ||||||
341.50 | 15.21 | ||||||
XA | 4.78 | 205.04 | 1 | 439.06 | 170.25* | 19.81 | 154.31 |
268.16 | 9.89 | ||||||
393.14 | 12.37 | ||||||
Kyn | 5.30 | 208.08 | 1 | 442.12 | 170.15* | 22.21 | 80.25 |
251.14 | 11.32 | ||||||
271.04 | 9.22 | ||||||
Trp | 5.38 | 203.80 | 1 | 438.18 | 170.89* | 23.33 | 122.21 |
200.02 | 17.63 | ||||||
283.56 | 16.51 | ||||||
5-HIAA | 6.22 | 191.06 | 1 | 425.11 | 171.15* | 22.39 | 240.83 |
205.89 | 19.33 | ||||||
380.35 | 12.54 | ||||||
KA | 6.51 | 189.04 | 1 | 423.51 | 170.44* | 18.72 | 120.39 |
252.10 | 11.65 | ||||||
378.22 | 12.25 | ||||||
5-HT | 7.75 | 179.06 | 2 | 643.34 | 171.13* | 37.95 | 88.75 |
380.10 | 15.66 | ||||||
393.02 | 28.77 | ||||||
CA (IS) | 7.78 | 182.06 | 2 | 647.09 | 171.11* | 27.39 | 145.28 |
234.57 | 20.72 | ||||||
413.07 | 18.70 |
Table 1 MS parameters of the target compounds
Compound | tR/min | Mr | Number of dansyl group | Precursor ion (m/z) | Product ion (m/z) | Collision energy/eV | RF lens |
---|---|---|---|---|---|---|---|
3-OH-Kyn | 3.86 | 224.08 | 2 | 691.14 | 171.14* | 37.54 | 98.31 |
456.15 | 27.48 | ||||||
349.37 | 14.98 | ||||||
3-OH-AA | 4.25 | 153.04 | 1 | 387.09 | 171.15* | 17.59 | 85.73 |
216.19 | 15.36 | ||||||
341.50 | 15.21 | ||||||
XA | 4.78 | 205.04 | 1 | 439.06 | 170.25* | 19.81 | 154.31 |
268.16 | 9.89 | ||||||
393.14 | 12.37 | ||||||
Kyn | 5.30 | 208.08 | 1 | 442.12 | 170.15* | 22.21 | 80.25 |
251.14 | 11.32 | ||||||
271.04 | 9.22 | ||||||
Trp | 5.38 | 203.80 | 1 | 438.18 | 170.89* | 23.33 | 122.21 |
200.02 | 17.63 | ||||||
283.56 | 16.51 | ||||||
5-HIAA | 6.22 | 191.06 | 1 | 425.11 | 171.15* | 22.39 | 240.83 |
205.89 | 19.33 | ||||||
380.35 | 12.54 | ||||||
KA | 6.51 | 189.04 | 1 | 423.51 | 170.44* | 18.72 | 120.39 |
252.10 | 11.65 | ||||||
378.22 | 12.25 | ||||||
5-HT | 7.75 | 179.06 | 2 | 643.34 | 171.13* | 37.95 | 88.75 |
380.10 | 15.66 | ||||||
393.02 | 28.77 | ||||||
CA (IS) | 7.78 | 182.06 | 2 | 647.09 | 171.11* | 27.39 | 145.28 |
234.57 | 20.72 | ||||||
413.07 | 18.70 |
Fig. 3 TIC chromatograms of the derivative products a. blank artificial urine sample; b. real urine sample; c. artificial urine spiked with standard solutions.Peak identifications: 1. Cr; 2. 3-OH-Kyn; 3. 3-OH-AA; 4. XA; 5. Kyn; 6. Trp; 7. 5-HIAA; 8. KA; 9. 5-HT; 10. CA (IS).
Compound | Linear equation | R2 | Linear range/ (μg/mL) | LOD/ (ng/mL) | Spiked content/ (μg/mL) | Recovery/% | RSDs (n=6)/% | |||
---|---|---|---|---|---|---|---|---|---|---|
Intra-day | Inter-day | |||||||||
3-OH-Kyn | Y=0.0082X-0.046 | 0.9764 | 0.1- | 5.0 | 0.01 | 0.1 | 105.41 | 1.31 | 0.61 | |
2.5 | 106.22 | 2.54 | 1.23 | |||||||
5 | 98.47 | 3.11 | 3.26 | |||||||
3-OH-AA | Y=0.0009X-0.0310 | 0.9873 | 0.5- | 25 | 0.1 | 0.5 | 93.24 | 0.78 | 0.78 | |
10 | 106.24 | 3.11 | 3.11 | |||||||
20 | 102.61 | 2.21 | 2.21 | |||||||
XA | Y=0.0645X -0.0683 | 0.9740 | 0.1- | 5.0 | 0.05 | 0.1 | 102.92 | 0.51 | 0.51 | |
2.5 | 104.23 | 2.14 | 2.14 | |||||||
5 | 96.97 | 1.16 | 1.16 | |||||||
Kyn | Y=2.9064X-0.1972 | 0.9941 | 0.5- | 25 | 0.1 | 1 | 95.96 | 1.23 | 1.23 | |
12 | 105.44 | 2.11 | 2.11 | |||||||
25 | 103.12 | 1.11 | 1.11 | |||||||
Trp | Y=0.5550X+0.1972 | 0.9954 | 1- | 50 | 0.5 | 2 | 107.65 | 2.14 | 3.59 | |
20 | 105.94 | 3.12 | 3.12 | |||||||
40 | 102.21 | 1.45 | 1.45 | |||||||
5-HIAA | Y=4.5184X+0.8491 | 0.9797 | 0.2- | 10 | 0.01 | 0.2 | 96.77 | 0.85 | 0.85 | |
4 | 104.33 | 2.33 | 2.33 | |||||||
8 | 107.25 | 2.54 | 2.54 | |||||||
KA | Y=0.0677X-0.0153 | 0.9908 | 0.1- | 5.0 | 0.05 | 0.1 | 96.77 | 0.75 | 0.75 | |
2 | 98.99 | 2.69 | 2.69 | |||||||
4 | 102.21 | 1.78 | 1.78 | |||||||
5-HT | Y=0.0105X+0.0457 | 0.9998 | 0.01- | 0.5 | 0.005 | 0.02 | 97.47 | 0.99 | 0.99 | |
0.25 | 104.43 | 1.23 | 1.23 | |||||||
0.5 | 103.32 | 1.25 | 1.25 |
Table 2 Linear equations, correlation coefficients (R2), linear ranges, LODs,recoveries and precisions of the target compounds
Compound | Linear equation | R2 | Linear range/ (μg/mL) | LOD/ (ng/mL) | Spiked content/ (μg/mL) | Recovery/% | RSDs (n=6)/% | |||
---|---|---|---|---|---|---|---|---|---|---|
Intra-day | Inter-day | |||||||||
3-OH-Kyn | Y=0.0082X-0.046 | 0.9764 | 0.1- | 5.0 | 0.01 | 0.1 | 105.41 | 1.31 | 0.61 | |
2.5 | 106.22 | 2.54 | 1.23 | |||||||
5 | 98.47 | 3.11 | 3.26 | |||||||
3-OH-AA | Y=0.0009X-0.0310 | 0.9873 | 0.5- | 25 | 0.1 | 0.5 | 93.24 | 0.78 | 0.78 | |
10 | 106.24 | 3.11 | 3.11 | |||||||
20 | 102.61 | 2.21 | 2.21 | |||||||
XA | Y=0.0645X -0.0683 | 0.9740 | 0.1- | 5.0 | 0.05 | 0.1 | 102.92 | 0.51 | 0.51 | |
2.5 | 104.23 | 2.14 | 2.14 | |||||||
5 | 96.97 | 1.16 | 1.16 | |||||||
Kyn | Y=2.9064X-0.1972 | 0.9941 | 0.5- | 25 | 0.1 | 1 | 95.96 | 1.23 | 1.23 | |
12 | 105.44 | 2.11 | 2.11 | |||||||
25 | 103.12 | 1.11 | 1.11 | |||||||
Trp | Y=0.5550X+0.1972 | 0.9954 | 1- | 50 | 0.5 | 2 | 107.65 | 2.14 | 3.59 | |
20 | 105.94 | 3.12 | 3.12 | |||||||
40 | 102.21 | 1.45 | 1.45 | |||||||
5-HIAA | Y=4.5184X+0.8491 | 0.9797 | 0.2- | 10 | 0.01 | 0.2 | 96.77 | 0.85 | 0.85 | |
4 | 104.33 | 2.33 | 2.33 | |||||||
8 | 107.25 | 2.54 | 2.54 | |||||||
KA | Y=0.0677X-0.0153 | 0.9908 | 0.1- | 5.0 | 0.05 | 0.1 | 96.77 | 0.75 | 0.75 | |
2 | 98.99 | 2.69 | 2.69 | |||||||
4 | 102.21 | 1.78 | 1.78 | |||||||
5-HT | Y=0.0105X+0.0457 | 0.9998 | 0.01- | 0.5 | 0.005 | 0.02 | 97.47 | 0.99 | 0.99 | |
0.25 | 104.43 | 1.23 | 1.23 | |||||||
0.5 | 103.32 | 1.25 | 1.25 |
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