Analysis and Purification of Bioactive Natural Products: The AnaPurNa Study

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1 Analysis and Purification of Bioactive Natural Products: The AnaPurNa Study Guido F. Pauli, *,, Shao-Nong Chen, J. Brent Friesen,, James B. McAlpine,, and Birgit U. Jaki, Department of Medicinal Chemistry and Pharmacognosy and Institute for Tuberculosis Research, College of Pharmacy, University of Illinois at Chicago, Chicago, IL 60612, United States Physical Sciences Department, Rosary College of Arts and Sciences, Dominican University, River Forest, IL 60305, United States Supporting Information page S1. Spectrum and Contribution of Survey Journals. S-1 S2. Survey Outcome: Number of Isolation Steps. S-2 S3. Correlation of Chromatographic Methodology Scores and the Number of Purification Steps S-3 S4. Distribution of Scores for General (A) and NMR (B) Spectroscopic Data. S-4 S5. Distribution of Scores for General Spectroscopic Data by Journal. S-5 S6. Distribution of Scores for NMR Spectroscopic Data by Journal. S-6 S7. Distribution of Spectroscopy Scores over Time. S-7 Supporting Information

2 S1. Spectrum and Contribution of Survey Journals. Graphical representation of the 13 surveyed journals and the number of articles contributed to the survey. The journal and their codes are as follows: Biological Pharmaceutical Bulletin (BPB), Chemical Pharmaceutical Bulletin (CPB), European Journal of Pharmacology (EJP), Fitoterapia (FIT), Journal of Ethnopharmacology (JETH), Journal of Natural Products (JNP), Journal of Pharmacy and Pharmacology (JPP), Journal of Pharmacology and Experimental Therapeutics (JPET), Phytochemi cal Analysiss (PCA), Phytochemistry (PC), Phytotherapy Research (PTR), Planta Medica (PM), Journal of Asian Natural Productss Research (JANPR) BPB CPB EJP FIT JETH JNP JPP JPET PCA PC PTR PM JANPR S-1

3 S2. Survey Outcome: Number of Isolation Steps. Graphical representation of the analysis of all surveyed articles for the maximum number of isolation steps used to purify the NPs prior to their biological evaluation. Extraction and liquid-liquid partitioning steps were not counted. The most elaborate scheme was a 10-step isolation process (1 report), followed by 8-step processes used in 3 studies. The value of 0 was assigned to the following studies: commercial sourcing or gifts; synthetic NPs; no purification was used at all or only extraction/partitioning was employed; obscure method reported. S-2

uses a log 2 vertical scale. The size of each sphere represents the frequency of occurrence of each data point.

4 S3. Correlation of Chromatographic Methodology Scores and the Number of Purification Steps. The scatter plot is based on data mined from all the articles surveyed in periods I, II and III (n tot = 1,823), and uses a log 2 vertical scale. The size of each sphere represents the frequency of occurrence of each data point. Insert B represents a zoomed and re-scaled version of insert A after omission of the data point for studies without reports of purification methods. A B S-3

5 S4. Distribution of Scores for General (A) and NMR (B) Spectroscopic Data. Proportions (%, y-axis) of scores (x-axis) given for all surveyed articles (n tot = 1,823), compounded for the three survey periods (I = , II = , II II = ). S-4

S5. Distribution of Scores for General Spectroscopic Data by Journal.

(top) and from the total score frequency data (bottom).

score frequency averages: 2.5 or lower in group A and 3.0 or higher in group B.

vertical axis cut at a maximum of 50. BPB CPB EJP FIT JET TH JNP JPP JPET PCA PC PTR PM JANPR score 2.

0 average score (% based) [avg eval periods!

35% 2 3% 20% 9% 10% 4% 0% 25% 37% 3% 15% 6% 3 88% 20% 55% 2% 88% 71% 50% 5% 67% 39% 1% 4 9% 26% 27%

6 S5. Distribution of Scores for General Spectroscopic Data by Journal. The table includes frequency and proportion of scores given for the surveyed articles (n tot = 1,823), sorted by journal. Percentages were calculated as averages of the proportions in each of the three evaluation periods (top) and from the total score frequency data (bottom). The latter were used to divide the journals into two groups based on the clear differences in total score frequency averages: 2.5 or lower in group A and 3.0 or higher in group B. Yellow and green highlighting marks values of 30 or greater for frequencies and percentages, respectively. The graphical representations visualize the distribution of scores for each journal, with the vertical axis cut at a maximum of 50. BPB CPB EJP FIT JET TH JNP JPP JPET PCA PC PTR PM JANPR score % 10% 9% 65% 8% 21% 18% 3% 10% 2% average score (% based) [avg eval periods!] 0% 4% 0% 14% 0% 0% 0% 5% 0% 7% 45% 1 score spec data: PERCENTAGE 0% 30% 9% 69% 8% 0% 25% 53% 7% 22% 35% 2 3% 20% 9% 10% 4% 0% 25% 37% 3% 15% 6% 3 88% 20% 55% 2% 88% 71% 50% 5% 67% 39% 1% 4 9% 26% 27% 5% 0% 29% 0% 0% 22% 17% 13% score spec data: FREQUENCY sum average score average of Group A journals average of Group B journals S-5

general spectroscopic data too divide the

Yellow and green highlighting marks values of

distribution of scores for each journal, with

3 2.4 54% 6% 2% 57% 12% 31% 21% 4% 11% 2% BPB

1 2.4 4.1 3.3 3. 8 2.5 3.9 4.1 3.0 2.3 4.1 3.5 2.

] 0% 0% 0% 5% 0% 0% 0% 4% 0% 0% 63% 1 score

71% 3% 26% 13% 2 0% 19% 5% 31% 13% 0% 0% 20%

41% 0% 4 9% 25% 5% 5% 4% 7% 0% 1% 22% 18% 25%

JANPR score 0 0 0 34 0 0 0 11 0 0 5 1 score

1 2 0 20 1 209 3 0 0 63 3 23 0 3 30 11 18 15

5 33 122 222 637 24 14 4 248 59 149 8 sum 4.

7 S6. Distribution of Scores for NMR Spectroscopic Data by Journal. The table includes frequency and proportion of scores given for the surveyed articles (n tot = 1,823), sorted by journal. Percentages were calculated as averages off the proportions in each of the three evaluation periods (top) and from the total score frequency dataa (bottom). The latter could equally be used like the general spectroscopic data too divide the journals into groups A and B (see S5). Yellow and green highlighting marks values of 30 or greater for frequencies and percentages, respectively. The graphical representations visualize the distribution of scores for each journal, with the vertical axis cut at a maximum of % 6% 2% 57% 12% 31% 21% 4% 11% 2% BPB CPB averag ge score (% based) [avg eval periods!] 0% 0% 0% 5% 0% 0% 0% 4% 0% 0% 63% 1 score NMR data: PERCENTAGE 0% 37% 9% 56% 0% 0% 50% 71% 3% 26% 13% 2 0% 19% 5% 31% 13% 0% 0% 20% 5% 15% 0% 3 91% 19% 82% 3% 83% 93% 50% 4% 69% 41% 0% 4 9% 25% 5% 5% 4% 7% 0% 1% 22% 18% 25% 5 EJP FIT JET TH JNP JPP JPET PCA PC PTR PM JANPR score score NMR data: FREQUENCY sum average score average of Group A journals average of Group B journals S-6

8 S7. Distribution of Spectroscopy Scores over Time. Separate graphs for general (A) and NMR (B) spectroscopic data show the distribution of the scores for all surveyed articles (n tot = 1,823), sorted by the three survey time periods I ( ), II ( ), and III ( ). S-7

Analysis and Purification of Bioactive Natural Products: The AnaPurNa Study

pubs.acs.org/jnp Analysis and Purification of Bioactive Natural Products: The AnaPurNa Study Guido F. Pauli,*,, Shao-Nong Chen, J. Brent Friesen,, James B. McAlpine,, and Birgit U. Jaki, Department of