Transcript Slide 1
Validating sequence assignments for peptide fragmentation patterns by Karen Jonscher www.proteomesoftware.com 503-244-6027 NEXT With the advent of high throughput proteomics, data is being generated at an astonishing rate. It has become clear that validating peptide sequence assignments generated by database search engines is an increasingly important, but often overlooked aspect of protein identification using tandem mass spectrometry. In this tutorial you will learn about some of the factors important in low energy peptide fragmentation and how to use this information to accept or reject database search engine peptide sequence assignments. NEXT Why is validating data important? These two fragment ion spectra from a multi-dimensional LC proteomics experiment using a quadrupole ion trap were searched with Mascot. They Every search, forequivalent? a variety of both had similar database scores. Are these two spectra • reasons, generates false positive Mascot and false Score = 101 negative assignments. We would like atspectrum High to quality good signal-toleast reduce, if not eliminate, these with incorrect noise and all of the dominant ions hits. assigned. • Decisions, often involving a great deal of money for bioassays, will be made Mascot Score = 102 downstream of our peptide identification. Inspectrum Poor quality with lowthe signal-tothis era of tight funding, it is crucial that noise. Fragment ions are mostrest likely data upon which these crucial decisions randomly assigned to are completely accurate. noise peaks. J L NEXT How do peptides break apart? In order to assess whether a sequence assignment is correct or not, it is important to understand how and why peptides break apart. Under low energy dissociation conditions, peptides primarily fragment at the C – N bond. If the charge is retained on the N-terminal end of the peptide, the ion is known as a b-type ion. If the charge is retained on the C-terminal end, the ion is termed a y-type ion. The fragmentation energy in some instruments, especially triple quadrupoles or quadrupole-time-of-flight hybrids (Q-TOFs) is often sufficient to generate cleavage at the C-C bond as well, causing loss of CO from the b ion. These ions are known as a-type ions. NEXT Peptides dissociate into nested sets of fragments H2N - b1 b2 b3 b4 A B C D y6 y5 y4 b5 E y3 b6 F y2 G - COOH y1 H2N-A+ =IfbA, y1 = +G-COOH 1 B, C, D, E, F and G represent +FG-COOH H2N-AB+different = b2 y = 2 amino acids, this peptide + H2N-ABC = b3 y3 = +EFG-COOH can dissociate to form the following + H2N-ABCD = b4 y4 = +DEFG-COOH fragments: + = b H2N-ABCDE y5 = +CDEFG-COOH 5 H2N-ABCDEF+ = b6 y6 = +BCDEFG-COOH H2N-ABCDEFG+ = b7 y7 = +ABCDEFG-COOH NEXT Mass difference reflects peptide sequence H2N - b1 b2 b3 b4 A B C D y6 y5 y4 b5 E y3 b6 F y2 G - COOH y1 Relative Abundance The peptide amino acid sequence can be deduced by calculating the difference in mass between peaks. If the mass corresponds to an amino acid residue (a table is shown in the next slide) then that amino acid is assigned to the peak representing the FG E D C B A difference. The largest y-type ion will appear 186 amu below the mass y2 anywhere between y4 57 to y 5 b2 y 3 of the precursor ion. The smallest y b ion will appear at the amino acid y6residue mass 3 b4 b5 plus 19 amu. The largest b ion will be at 18 amu plus the residueb mass below the 6 precursor and the smallest b ion AB C will be at the D residue E mass +F1. G Using this information, we can interpret fragmentation spectra to deduce the amino m/z acid sequence. Keep clicking to view an ion series. NEXT basic Name Symbol Mass (-H2O) Side Chain Immonium/Related Ions Alanine A, Ala 71.079 CH3- 44 Arginine R, Arg lose ammonia156.188 HN=C(NH2)-NH-(CH2)3- 129/59, 70. 73, 87, 100, 112 H2N-CO-CH2- 87/70 HOOC-CH2- 88/70 HS-CH2- 76 H2N-CO-(CH2)2- 101 Asparagine acidic Aspartic acid -H2S=34 Cysteine Glutamine acidic Glutamic acid Glycine basic Histidine Isoleucine Leucine basic Lysine Not observed lose ammonia N, Asnusually 114.104 inD, ion traps due to low mass Asp 115.089 cutoff. Same with b1/y1. C, Cys 103.145 Q, Gln lose ammonia128.131 The table of common amino acids suppress b provides molecular weights for the residues, structures of the side chains, isobaric and masses for the low mass immonium isobaric ions thatlose result from side chain loss. ammonia -CH3SH=48 Methionine E, Glu 129.116 HOOC-(CH2)2- pro102/56, 84, 129 G, Gly 57.052 H- 30 H, His 137.141 N=CH-NH-CH=C-CH2|__________| 110/82, 121, 123, 138, 166 I, Ile 113.160 CH3-CH2-CH(CH3)- 86/44, 72 L, Leu 113.160 (CH3)2-CH-CH2- 86/44, 72 K, Lys 128.17 H2N-(CH2)4- 101/70, 84, 112, 129 M, Met 131.199 CH3-S-(CH2)2- 104/61 These amino acids have chemical suppress b typically dominant properties that need to be considered when validating sequence assignments. Phenylalanine F, Phe 147.177 Phenyl-CH2- 120/91 Proline P, Pro 97.117 -N-(CH2)3-CH- |_________| 70 S, Ser 87.078 HO-CH2- 60 lose waterThreonine T, Thr 101.105 CH3-CH(OH)- 74 Tryptophan W, Trp 186.213 Phenyl-NH-CH=C-CH2|___________| 159/77, 117, 130, 123, 170, 171 Tyrosine Y, Tyr 163.176 4-OH-Phenyl-CH2- 136/91, 107 Valine V, Val 99.133 CH3-CH(CH2)- 72/41, 55, 69 lose water Serine abundant y NEXT Other things to keep in mind Basic amino acids can generate doubly-charged ions. Ion signal can be intense for cleavages C-terminal to acidic amino acids. These residues also tend to lose water and cyclize to randomly eject portions of the sequence. Isobaric amino acids cannot be differentiated using low energy fragmentation instruments. Loss of water from threonine is particularly intense if the amino acid is near a terminal end of the peptide. If a peptide is tryptic, y1 will either be lysine at 147 or arginine at 175. Some pairs of amino acids add up to the mass of a different amino acid. The same can happen with acetylated amino acids, a common modification. G-G = 114 = N G-A = 128 = K/Q V-G = 156 = R G-E = 186 = W A-D = 186 = W S-V = 186 = W AcG = 99 = V AcA = 113 = L/I AcS = 129 = E AcN = 156 = R NEXT Lxx Val Val Phe K/Q Gly Arg We’re going to manually interpret an MS/MS spectrum generated by a quadrupole ion trap. 1219.4 1337.5 1276.5 1238.6 1139.4 1091.4 992.4 The The firstdeconvoluted ion is at 1337.5. mass 1450- of the precursor is 1449.38 (the observed 1337=113=Lxx, therefore we assign the ion was doubly charged). largest y ion as either leucine or isoleucine. We’ll start byion looking the dominant peaks that are below the mass Next we look at the at 1238.atAssuming it is a The y of ion,next we ion note 1337-1238=99=Val, so we is that at 1276. 1450-18the precursor ion. assign the next y ion as Val.we assign the 1276=156=Arg, therefore largest b ion as arginine. Since the sample We’ll lookwith for trypsin, possible y ions between 57 and 186 amu below 1450 was digested we would expect Continuing in this+ manner, weypossible find (theor(M+H) ion) b ions in a window offset by another lysine arginine as theand first ion.b ions at 1276-1219=57=Gly and 18 amu. 1219-1091=128=Lys/Gln and y ions at 1238-1139=99=Val and 1139992=147=Phe. NEXT Lxx Val Val Phe K/Q Gly Arg 863.4 To verify the high mass y ion assignments, we look forSince thethe largest y ion was either leucine or complimentary low massisoleucine b ions. and the next y ion in the series 1219.4 360.2 992.4 was valine, we look for the complementary ion at 113+1+99=213=b2. Since the data is from an ion trap, we The next b ion will result from addition of will probably not see b1. another valine, therefore we’d expect a signal at 213+99=312=b3. 1337.5 1276.5 1139.4 4 1238.6 927.3 944.3 975.4 443.3 459.0 213.0 311.8 232.0 ion at 312+147=459. 1091.4 Therefore, we start byWhen looking for b2. is added, we find the b phenylalanine NEXT Lxx Val Val Phe K/Q Q Gly Arg To verify the high mass b ion assignments, we look for the complimentary low mass y ions. 863.4 Assuming arginine is y1, we look for a signal resulting from the addition of glycine at Since the data is from156+1+18+57=232=y an ion trap, we 2. We add the 19 amu to The next complementary y ion should be will probably not see account y1, however the group. the carboxyl atfor 232+128=360=y resulting from the 3 1337.5 1276.5 1238.6 927.3 944.3 975.4 443.3 459.0 311.8 1139.4 1091.4 lysine, since we would have expected a cleavage there. Therefore, we start by looking for y2. 232.0 213.0 1219.4 360.2 992.4 assignment of arginine makes sense addition of either lysine or glutamine. the sample was digested using given that the sample was Since digested trypsin, it is unlikely that the amino acid is using trypsin. NEXT Lxx Val Val Phe Glu Asn Phe Gln Gly Arg 863.4 507.2 We look for the next largest b ion below 1091. our There Validating high mass ion assignments, we expect to find b5 are three choices: resulting from addition of glutamic acid at 459+129=588=b5 and The next dominant peak should correspond to a b ion y resulting from addition of phenylalanine, 360+147=507=y4. so we look ybelow 944 and note that992 9444 Since 992The next largest ion will appear below 1091-975=116 830=114=Asn. 863=129=Glu, we assign the next y ion as glutamic acid. 1091-944=147=Phe 1091-975=116 1091-944=147=Phe 1091-927=164 1337.5 1276.5 1238.6 1139.4 1091.4 992.4 927.3 944.3 975.4 543.3 489.0 b4 b2 443.3 b3 y2 588.0 830.2 y3 Only the signal at 944 corresponds to an amino acid residue mass, therefore the next b ion is Phe. 1219.4 1091-927=164 NEXT Glu Asn Phe Gln Gly Arg 750.3 Lxx Val Val Phe Glu Lxx 621.3 863.4 1219.4 1337.5 1276.5 1238.6 1139.4 1091.4 992.4 830.2 701.1 927.3 944.3 975.4 b5 543.3 489.0 b4 b2 443.3 b3 y2 y3 y4 The next largest y ion will appear below 863. Since 863-750=113=Lxx, we assign the next y ion as leucine/isoleucine. The next dominant peak should correspond to a b ion so we look below 830 and note that 830701=129=Glu. The next y ion will appear below 750. Since 750621=129=Glu, we assign the next y ion as glutamic acid. However, since this is complementary to the b ion we just assigned, our sequence is complete. 1091-975=116 1091-944=147=Phe 1091-927=164 NEXT b V V F E L E N F Q G R y y5 L y11 b11 y10 b8 b5 543.3 489.0 b4 b2 443.3 b3 y2 b9 y9 b7 y3 y8 b10 b5 y7 y4 y6 In this example we have observed a complete series of complementary b and y ions. Purple bars indicate b ions while orange bars are for y ions. 1091-975=116 1091-944=147=Phe 1091-927=164 NEXT Incorrect Identification # Rank/Sp --- -------1. 1 / 1 2. 2 / 2 3. 3 / 2 4. 4 / 3 5. 5 / 6 6. 6 / 5 7. 7 / 13 8. 8 / 13 9. 9 / 15 10. 10 / 11 11. 11 / 16 12. 12 / 4 Id# -------0 0 0 0 0 0 0 0 0 0 0 0 (M+H)+ deltCn XCorr Sp Ions Reference Peptide ------------- matches -----------------to ------Sequest tenatively each---spectrum 1450.7694 0.0000 4.7567 2559.1 20/22 CRB1_HUMAN R.LVVFELENFQGR.R 12 peptides. are 2541.5 rated 20/22 with the Xcorr R.LVVFELEN*FQGR.R 1451.7534 Matches 0.0254 4.6357 CRB1_HUMAN 0.0571 4.4851 2541.5 20/22 CRB1_HUMAN R.LVVFELENFQ*GR.R value 1451.7534 (Sequest’s score criterion). HereCRB1_HUMAN is a 1452.7374 0.2804 3.4230 2036.0 18/22 R.LVVFELEN*FQ*GR.R 1451.7569 0.4038 2.8358 1057.7 15/22 TP3B_HUMAN K.LN*M#VKFLQ*VEGR.G poorly1450.7729 rated match. Although most of the 0.4619 2.5595 1426.3 17/22 TP3B_HUMAN K.LN*M#VKFLQVEGR.G 1450.6549 840.0they 13/22were NEUM_HUMAN dominant ions 0.4654 were 2.5430 assigned, not R.TKQ*VEKN*DDDQ*K.I 1449.6709 0.4752 2.4964 840.0 13/22 NEUM_HUMAN R.TKQ*VEKNDDDQ*K.I 1449.6709 817.4 13/22 NEUM_HUMAN assigned to b 0.4757 and y 2.4941 ions but to water loss and R.TKQ*VEKN*DDDQK.I 1451.7055 0.5042 2.3586 843.6 13/22 ING_HUMAN K.S]VETIKEDM#NVK.F other ions that0.5145 are generally less14/22 abundant. 1451.8011 2.3093 817.3 GGT5_HUMAN R.VNVYHHLVETLK.F 1451.7494 0.5179 2.2932 1458.5 16/20 DESP_HUMAN R.LTYEIEDEKRR.R NEXT Correct Identification # Rank/Sp --- -------1. 1 / 1 2. 2 / 2 3. 3 / 2 4. 4 / 3 5. 5 / 6 6. 6 / 5 7. 7 / 13 8. 8 / 13 9. 9 / 15 10. 10 / 11 11. 11 / 16 12. 12 / 4 Id# -------0 0 0 0 0 0 0 0 0 0 0 0 (M+H)+ deltCn -------- -----1450.7694 0.0000 1451.7534 0.0254 1451.7534 0.0571 1452.7374 0.2804 1451.7569 0.4038 1450.7729 0.4619 1450.6549 0.4654 1449.6709 0.4752 1449.6709 0.4757 1451.7055 0.5042 1451.8011 0.5145 1451.7494 0.5179 XCorr -----4.7567 4.6357 4.4851 3.4230 2.8358 2.5595 2.5430 2.4964 2.4941 2.3586 2.3093 2.2932 Sp ---2559.1 2541.5 2541.5 2036.0 1057.7 1426.3 840.0 840.0 817.4 843.6 817.3 1458.5 Ions Reference Peptide ---- --------------20/22 CRB1_HUMAN R.LVVFELENFQGR.R 20/22 CRB1_HUMAN R.LVVFELEN*FQGR.R 20/22 CRB1_HUMAN R.LVVFELENFQ*GR.R 18/22 CRB1_HUMAN R.LVVFELEN*FQ*GR.R 15/22 TP3B_HUMAN K.LN*M#VKFLQ*VEGR.G 17/22 TP3B_HUMAN K.LN*M#VKFLQVEGR.G 13/22 NEUM_HUMAN R.TKQ*VEKN*DDDQ*K.I 13/22 NEUM_HUMAN R.TKQ*VEKNDDDQ*K.I 13/22 NEUM_HUMAN R.TKQ*VEKN*DDDQK.I 13/22 ING_HUMAN K.S]VETIKEDM#NVK.F 14/22 GGT5_HUMAN R.VNVYHHLVETLK.F 16/20 DESP_HUMAN R.LTYEIEDEKRR.R When we compare the incorrect with the correct identification, we see that all of the dominant ions are assigned to b and y ions, with water losses accounting for many of the lower abundance peaks. The rank is 1 and the Xcorr is high in the Sequest output file for the correct ID. NEXT Score vs. Spectral Quality As we have seen, a high score may be an indicator that an identification is correct. Good Spectral Quality Good Score However, this does not hold true in all Bad ID Bad ID cases. In the next few examples, we will Good IDsee Good ID instances where good scores actually corresponded to bad identifications, and bad scores corresponded to good identifications. Bad Score ? ID The importance of spectral quality is demonstrated and the case of questionable identification Bad ID is reviewed. Bad ID Bad Spectral Quality NEXT Example 1 Proteomics Data Mascot Search Good Spectral Quality Bad ID Bad Score Good Score Bad Spectral Quality NEXT Great score, nice spectrum The mass spectrum has a lot of 1. IPI00001661 Mass: 45425 Total score: 111 Peptides matched: 1 fragment ions and has good Tax_Id=9606 Regulator of chromosome condensation Check to include this hit in error signal to noise. Oftentimes, tolerant search or archive report good quality spectra like this Query Observed Mr(expt) Mr(calc) Delta Miss Score Rank Peptide provide good search results. 1 950.77 1899.53 1899.00 0.53 0 111 1 The Mascot score is 111. Usually, scores over 40 or 50 typically generate correct identifications. VVQVSAGDSHTAALTDDGR The score is well beyond the 95% confidence level and is well separated from the other possibilities, generally a positive indicator of a correct ID. NEXT The masses of the expected sequence ions are summarized in the data table. Masses labeled in red were observed in the experiment. As we can see, we have a fairly long run of contiguous sequence for the y ions and a shorter run for the b ions. There is some overlap of ++ 0++ # b++ b* b*so b0 Seq. y y++ y* y*++ y0 y0++ # the b band y ions, however, we have a bcomplementary set. 1 100.14 50.57 V 2 199.27 100.14 V 1800.88 900.94 1783.85 892.43 1782.87 891.94 18 3 327.40 164.21 310.37 155.69 Q 1701.75 851.38 1684.72 842.86 1683.73 842.37 17 4 426.54 213.77 409.51 205.26 V 1573.62 787.31 1556.59 778.80 1555.60 778.30 16 5 513.61 257.31 496.58 248.80 495.60 248.30 S 1474.48 737.75 1457.45 729.23 1456.47 728.74 15 6 584.69 292.85 567.66 284.34 566.68 283.84 A 1387.41 694.21 1370.38 685.69 1369.39 685.20 14 7 641.75 321.38 624.72 312.86 623.73 312.37 G 1316.33 658.67 1299.30 650.15 1298.31 649.66 13 8 756.83 378.92 739.80 370.41 738.82 369.91 D 1259.28 630.14 1242.24 621.63 1241.26 621.13 12 9 843.91 422.46 826.88 413.94 825.90 413.45 S 1144.19 572.60 1127.16 564.08 1126.17 563.59 11 10 981.05 491.03 964.02 482.52 963.04 482.02 H 1057.11 529.06 1040.08 520.54 1039.09 520.05 10 11 1082.16 541.58 1065.13 533.07 1064.14 532.58 T 919.97 460.49 902.94 451.97 901.95 451.48 9 12 1153.24 577.12 1136.21 568.61 1135.22 568.12 A 818.86 409.94 801.83 401.42 800.85 400.93 8 13 1224.32 612.66 1207.29 604.15 1206.30 603.65 A 747.78 374.40 730.75 365.88 729.77 365.39 7 14 1337.48 669.24 1320.45 660.73 1319.46 660.23 L 676.70 338.86 659.67 330.34 658.69 329.85 6 15 1438.58 719.79 1421.55 711.28 1420.57 710.79 T 563.55 282.28 546.51 273.76 545.53 273.27 5 16 1553.67 777.34 1536.64 768.82 1535.65 768.33 D 462.44 231.72 445.41 223.21 444.42 222.72 4 17 1668.76 834.88 1651.73 826.37 1650.74 825.88 D 347.35 174.18 330.32 165.66 329.34 165.17 3 18 1725.81 863.41 1708.78 854.89 1707.79 854.40 G 232.26 116.64 215.23 108.12 2 R 175.21 88.11 158.18 79.59 1 19 19 NEXT Despite the many of the factors which seemed to lead to a correct identification, it is wrong. Since this is a good quality spectrum, it would be worth pursuing other interpretation options. For one, the peptide may be modified and it would be worth re-searching the data using a database including modifications such as phosphorylation or glycosylation, among others. Several searches may be required. De novo searching would also be a possible approach if modification Can’t account for dominant searches do not provide acceptable results. ions!!! Incorrect ID BUT… NEXT Example 2 Good Spectral Quality Bad ID Bad Score Good Score Bad Spectral Quality NEXT All dominant ions are unidentified, the spectrum is of good quality, with good signal to noise and well-separated fragment ions Mascot score is below generally accepted thresholds. No significant hits to report Unassigned queries: (no details means no match) Query Observed Mr(expt) Mr(calc) Delta Miss Score Rank Peptide 1 868.07 1734.13 1730.98 3.15 2 29 1 KGVASTDNTLIARSLGK NEXT There are only short runs of contiguous sequence, there is little complementarity between the b and y ions. With dominant ions unidentified the assignment is obviously incorrect. Since the spectrum is of good quality, the next step should be to consider modifications. # b b++ b* b*++ 1 129.18 65.10 112.15 56.58 K 2 186.23 93.62 169.20 85.11 G 1603.82 802.41 1586.79 793.90 1585.80 793.40 16 3 285.37 143.19 268.34 134.67 V 1546.76 773.89 1529.73 765.37 1528.75 764.88 15 4 356.45 178.73 339.42 170.21 A 1447.63 724.32 1430.60 715.80 1429.62 715.31 14 5 443.52 222.27 426.49 213.75 425.51 213.26 S 1376.55 688.78 1359.52 680.27 1358.54 679.77 13 6 544.63 272.82 527.60 264.30 526.61 263.81 T 1289.48 645.24 1272.44 636.73 1271.46 636.23 12 7 659.72 330.36 642.69 321.85 641.70 321.36 D 1188.37 594.69 1171.34 586.17 1170.35 585.68 11 8 773.82 387.41 756.79 378.90 755.81 378.41 N 1073.28 537.14 1056.25 528.63 1055.27 528.14 10 9 874.93 437.97 857.90 429.45 856.91 428.96 T 959.18 480.09 942.15 471.58 941.16 471.09 9 10 988.09 494.55 971.06 486.03 970.07 485.54 L 858.07 429.54 841.04 421.02 840.06 420.53 8 11 1101.25 551.13 1084.21 542.61 1083.23 542.12 I 744.91 372.96 727.88 364.45 726.90 363.95 7 12 1172.32 586.67 1155.29 578.15 1154.31 577.66 A 631.75 316.38 614.72 307.87 613.74 307.37 6 13 1328.51 664.76 1311.48 656.24 1310.50 655.75 R 560.67 280.84 543.64 272.33 542.66 271.83 5 14 1415.59 708.30 1398.56 699.78 1397.57 699.29 S 404.49 202.75 387.46 194.23 386.47 193.74 4 15 1528.75 764.88 1511.72 756.36 1510.73 755.87 L 317.41 159.21 300.38 150.69 3 16 1585.80 793.40 1568.77 784.89 1567.79 784.40 G 204.25 102.63 187.22 94.11 NEXT 2 K 147.20 74.10 130.17 65.59 1 17 b0 b0++ Seq. y y++ y* y*++ y0 y0++ # 17 Example 3 Good Spectral Quality Good ID Bad Score Good Score Bad Spectral Quality NEXT Score = 31 below threshold BUT… All dominant ions accounted for Largest peak corresponds to y5 – cleavage at proline # b b0 Seq. 1 72.09 A 2 129.14 G y y* y0 # 15 1391.57 14 3 186.19 1352.53 1335.50 1334.52 •Chemistry isG plausible 4 257.27 A 1295.48 1278.45 1277.46 Sequest search provided Water loss for y ions also starts after•A 5 328.35 A 1224.40 1207.37 1206.38 the threonine. 6 427.48 V 1153.32 1136.29as 1135.31 the same identification 7 526.61 V 1054.19 1037.16 1036.17 Possibly the presence of the basic the Mascot search histidine and the acidic glutamic acid 8 639.77 I 955.06 938.03 937.04 correct assignment inhibit the water loss at y and y . •Likely 9 740.88 722.86 T 841.90 824.87 823.88 13 No water loss for b ions until b9 when Thr appears. 3 1409.58 1392.55 12 11 10 4 9 8 7 10 869.99 851.98 E 740.79 723.76 722.78 6 11 967.11 949.10 P 611.68 594.65 593.66 5 12 1096.23 1078.21 E 514.56 497.53 496.54 4 13 1233.37 1215.35 H 385.44 368.41 367.43 3 14 1334.47 1316.46 T 248.30 231.27 230.29 2 K 147.20 130.17 15 1 NEXT Example 4 Good Spectral Quality Bad Score Good Score Bad ID Bad Spectral Quality NEXT Score = 18 Very weak spectrum There is no baseline, thus we must assume this is a noise spectrum. The ions are likely assigned by random chance. NEXT # b b++ 1 58.06 29.53 2 157.19 79.10 3 228.27 114.64 4 299.35 150.18 5 412.51 206.76 6 513.61 257.31 7 600.69 300.85 8 715.78 358.39 9 812.90 406.95 10 883.98 442.49 11 983.11 492.06 12 1111.24 556.12 13 1182.32 14 Although there are some complementary runs of contiguous sequence ions, it is unlikely they are significant, given the quality of the mass spectrum. b* b*++ b0 b0++ Seq. y y++ y* y*++ y0 y0++ G 495.60 248.30 # 25 V 2413.73 1207.37 2396.70 1198.85 2395.71 1198.36 24 A 2314.60 1157.80 2297.57 1149.29 2296.58 1148.79 23 A 2243.52 1122.26 2226.49 1113.75 2225.50 1113.25 22 L 2172.44 1086.72 2155.41 1078.21 2154.42 1077.72 21 T 2059.28 1030.14 2042.25 1021.63 2041.26 1021.14 20 We do see a dominant fragment ion at the y17 proline, however other large signals do not correspond to expected cleavages C-terminal of the acidic amino acids. 582.68 291.84 S 1958.17 979.59 1941.14 971.08 1940.16 970.58 19 697.77 349.39 D 1871.10 936.05 1854.06 927.54 1853.08 927.04 18 794.88 397.95 P 1756.01 878.51 1738.98 869.99 1737.99 869.50 17 865.96 433.48 A 1658.89 829.95 1641.86 821.43 1640.87 820.94 16 965.09 483.05 V 1587.81 794.41 1570.78 785.89 1569.80 785.40 15 1094.21 547.61 1093.23 547.12 Q 1488.68 744.84 1471.65 736.33 1470.66 735.84 14 591.66 1165.29 583.15 1164.30 582.66 A 1360.55 680.78 1343.52 672.26 1342.53 671.77 13 1295.48 648.24 1278.45 639.73 1277.46 639.24 I 1289.47 645.24 1272.44 636.72 1271.45 636.23 12 15 1394.61 697.81 16 1507.77 754.39 17 1622.86 811.93 18 1723.96 862.49 19 1795.04 898.03 20 1882.12 941.56 21 1997.21 22 The assignment of doubly-charged ions without the presence of a basic ion is highly unlikely, therefore this identification is incorrect. 1377.58 689.29 1376.60 688.80 V 1176.31 588.66 1159.28 580.14 1158.29 579.65 11 1490.74 745.87 1489.76 745.38 L 1077.18 539.09 1060.15 530.58 1059.16 530.08 10 1605.83 803.42 1604.84 802.93 D 964.02 482.51 946.99 474.00 946.00 473.51 9 1706.93 853.97 1705.95 853.48 T 848.93 424.97 831.90 416.45 830.91 415.96 8 1778.01 889.51 1777.03 889.02 A 747.82 374.42 730.79 365.90 729.81 365.41 7 1865.09 933.05 1864.11 932.56 S 676.74 338.88 659.71 330.36 658.73 329.87 6 999.11 1980.18 990.59 1979.19 990.10 D 589.67 295.34 572.64 286.82 571.65 286.33 5 2096.34 1048.68 2079.31 1040.16 2078.33 1039.67 V 474.58 237.79 457.55 229.28 456.56 228.79 4 23 2209.50 1105.26 24 2324.59 1162.80 25 This spectrum could likely be discarded. 2192.47 1096.74 2191.49 1096.25 L 375.45 188.23 358.42 179.71 357.43 179.22 3 2307.56 1154.28 2306.58 1153.79 D 262.29 131.65 245.26 123.13 244.27 122.64 2 K 147.20 74.10 130.17 65.59 NEXT 1 Example 5 Good Spectral Quality Good Score ? ID Bad Spectral Quality Bad Score NEXT Scorebelow = 38 threshold, spectral quality OK but Score slightly fragmentation is limited, questionable ID Most abundant peak results from loss of water The identification could possibly be disregarded if the protein from serine, not proline assignment was confirmed by another peptide. cleavage as expected. The doubly-charged y8 ion is reasonable, given the presence of the arginine. However, the b2 doubly-charged ion is unlikely. # b b++ 1 132.20 66.60 2 261.32 131.16 243.30 122.15 E 945.06 473.04 928.03 464.52 927.05 464.03 8 3 358.43 179.72 340.42 170.71 P 815.95 408.48 798.92 399.96 797.93 399.47 7 4 472.54 236.77 455.51 228.26 454.52 227.76 N 718.83 359.92 701.80 351.40 700.82 350.91 6 5 559.61 280.31 542.58 271.80 541.60 271.30 S 604.73 302.87 587.70 294.35 586.71 293.86 5 6 672.77 336.89 655.74 328.38 654.76 327.88 L 517.65 259.33 500.62 250.81 499.63 250.32 4 7 828.96 414.98 811.93 406.47 810.95 405.98 R 404.49 202.75 387.46 194.23 386.47 193.74 3 8 930.07 465.54 913.04 457.02 912.05 456.53 T 248.30 124.66 231.27 116.14 230.29 115.65 2 K 147.20 74.10 130.17 65.59 9 b* b*++ b0 b0++ Seq. y y++ y* y*++ y0 y0++ # M 9 NEXT 1 Example 6 Good Spectral Quality Good ID Bad Score Good Score Bad Spectral Quality NEXT Score = 79 Complete b and y series Plausible ion chemistry Correct ID! Abundant ions at D and W cleavages # b b++ b* b*++ b0 b0++ Seq. y y++ y* y*++ y0 y0++ 1 132.20 66.60 2 233.31 117.16 215.29 108.15 T 1689.83 845.42 1672.79 836.90 1671.81 836.41 13 3 348.39 174.70 330.38 165.69 D 1588.72 794.86 1571.69 786.35 1570.71 785.86 12 4 476.52 238.77 459.49 230.25 458.51 229.76 Q 1473.63 737.32 1456.60 728.80 1455.62 728.31 11 5 605.64 303.32 588.61 294.81 587.63 294.32 E 1345.50 673.25 1328.47 664.74 1327.49 664.25 10 6 676.72 338.86 659.69 330.35 658.70 329.86 A 1216.39 608.70 1199.35 600.18 1198.37 599.69 9 7 789.88 395.44 772.85 386.93 771.86 386.44 I 1145.31 573.16 1128.28 564.64 1127.29 564.15 8 8 918.01 459.51 900.98 450.99 899.99 450.50 Q 1032.15 516.58 1015.12 508.06 1014.13 507.57 7 9 1033.10 517.05 1016.07 508.54 1015.08 508.05 D 904.02 452.51 886.99 444.00 886.00 443.50 6 10 1146.26 573.63 1129.23 565.12 1128.24 564.63 L 788.93 394.97 771.90 386.45 5 11 1332.47 666.74 1315.44 658.22 1314.46 657.73 W 675.77 338.39 658.74 329.87 4 12 1460.60 730.80 1443.57 722.29 1442.59 721.80 Q 489.55 245.28 472.52 236.77 3 13 1646.82 823.91 1629.78 815.40 1628.80 814.90 W 361.42 181.22 344.39 172.70 NEXT2 R 175.21 88.11 158.18 79.59 1 14 M # 14 The following examples compare spectra that were acquired on a Q-TOF and an ion trap. Both correct and incorrect identifications are shown. The different appearance of the fragmentation spectra, and the presence of immonium ions and low mass fragment ions in the Q-TOF, means that different considerations may need to be taken into account when different instruments are being used. NEXT Correct Identification Note the presence of y1 and the immonium ion for F in the QTOF spectrum. The QTOF spectrum shows b ion suppression except for b2. QTOF Ion Trap NEXT Incorrect Identification Both spectra have many dominant ions unaccounted for. The dominant ions are assigned as b type in the QTOF spectrum, which is unlikely. QTOF Ion Trap NEXT Look at the next two slides. Can you guess which are the correct identifications and which are incorrect? NEXT QTOF Ion Trap NEXT QTOF Ion Trap NEXT Summary When interpreting the results of search engines it is important to – Look at the score – Look at the sequence runs – Consider the ion fragmentation chemistry – What about the instrument? – Does it all make sense? www.proteomesoftware.com