This hyphenated technique shows the promising results for the analysis of small combinatorial libraries containing up to molecules. Common derivatization method is the conversion of the component to trimethylsilyl, acetyl, and methyl derivatives.But, on hydrolysis, and acetylation of active fraction followed by GCMS analysis, only two peaks were identied as phorbol tetraacetates by comparison with phorbol triacetate. Since a lot of organic compounds produce peaks at characteristic wavelengths, FTIR is a useful detection technique.But, due to the presence of solvents producing intense peaks in the same region, this technique is much less sensitive than other detection methods like UV and MS.HPLC separation followed by NMR analysis is a potential technique for the investigation of natural products. HPLCSPENMR has an important advantage over HPLCNMR in that the compounds are accumulated on SPE cartridges by repetitive adsorption.Further, the analytes are extracted by deuterated solvent, so that compounds are concentrated in detection cells, resulting in increased sensitivity of this hyphenated technique. The extract was submitted to online LCNMR to conrm the above ndings and to obtain more structural data.Compound was conrmed as decussatin, and compound, responsible for antifungal activity, was nally identied as the known methoxy, naphthoquinone. Optimization also requires modifying, replacing, or adding functional groups and stereo centers or extreme remodeling of the fundamental scaffold to optimize physicochemical and pharmacokinetic properties.Thus, natural products are guiding principles or natural productbased design and synthesis of compound libraries. The application of synthetic chemistry to modify the leads of the natural product has long been used to produce compounds with improved pharmacological properties.This semisynthetic approach has been widely used either to generate more similar compounds randomly or to improve lead natural product candidates. For example, aspirin is the best and rst example; it was synthesized from salicin.Similarly, the cholesterol lowering semisynthetic simvastatin is more potent than parent lovastatin. Taxol is one of the most effective anticancer drugs ever developed.Similarly, camptothecin was identied as potent anticancer agent; later the solubility issue was resolved by semisynthesizing potent anticancer compounds topotecan and irinotecan that are widely used for cancer treatment.There are a Targetmol’s Benzethonium chloride number of potential candidates of natural origin used for semisynthesisbased natural product libraries.One of the excellent examples of natural product inspired total synthesis is the discovery of avopiridol. Rohitukine was isolated as the constituent accounting for antiinammatory and immunomodulatory activity.Hyphenated techniquesbased dereplication and early identication of known compounds in crudefraction combined with bioassayguided fractionation drastically enhanced the drug discovery outcomes.LCMS is now considered as a major hyphenated technique widely used in academia and industry.This technique gained immense popularity in the last years, and hence the creation of databases or repository of MSMS fragmentbased mass spectrometry data has gained popularity in the eld of natural products dereplication.The standard MSMS fragmentation of a particular metabolite remains same under the same experimental conditions which can be considered as a signature or ngerprint of that particular metabolite.These signature proles help in the identication of known metabolites within the crude.These plants possess a wide range of bioactive principles which alone or synergistically act on different targets.