Of lack-of-fit test (self-assurance level at 95 ). d The LOD was defined because the concentration for which the signal-to-noise ratio was three; the LOQ was defined as the concentration for which the signal-to-noise ratio was 10.TablePrecision, repeatability and stability information of 10 analytes (RSD , n ).Precision Inter-day Retention time Peak area 1.9 1.1 1.7 1.7 two.0 1.9 0.9 1.3 1.1 1.0 Intra-day Retention time 0.five 0.eight 0.9 0.7 0.five 0.four 0.3 0.five 0.4 0.6 Peak location 1.2 0.7 1.four 1.0 1.four 1.three 1.0 1.six 0.9 0.7 Retention time 0.7 1.1 0.9 1.four 1.six 1.five 0.6 1.2 0.8 1.1 Content material 1.8 1.6 1.five 1.7 two.1 1.7 2.0 two.two 1.9 1.six Retention time 0.four 0.five 0.four 0.six 0.three 0.six 0.five 0.7 0.4 0.six Peak area 0.eight 1.two 0.9 1.3 1.4 1.two 0.9 0.8 1.5 1.1 Repeatability StabilityCompoundProtopine Jatrorrhizine Coptisine Palmatine Berberine Xanthotoxin Bergapten Tetrahydropalmatine Imperatorin Isoimperatorin0.4 0.five 0.7 0.six 0.5 0.6 0.5 0.4 0.four 0.three.five.Qualitative analysis of widespread peaksThirty-three frequent peaks described in the fingerprint chromatogram which includes 10 quantitative compounds were identified or tentatively characterized, and their ESI-MS/MS information and fragmentations are listed in Table 6. 3.5.1. Identification of fifteen alkaloids from Rhizoma Corydalis For protopine and tetrahydroprotoberberine alkaloids, their characteristic fragmentation pathway was Retro-Diels lder (RDA) rupture [14]. Compound 3 gave protonated molecular ion [M�H](m/z 354) in positive-ion mode. The RDA rupture from [M�H]may create fragment ions at m/z 149 and m/z 206. The fragment ion at m/z 189 could be as a result of loss of OH in the fragment ion at m/z 206. By comparing the UV and MS spectra with these on the reference typical, compound three was unequivocally identified as protopine [10,14].Palladium(II) chloride Formula Similarly, compound four yielded [M�H]at m/z 370 as well as a series of ions like [M�H-C10H12O2]at m/z206, [M�H-C10H12O2-H2O]at m/z 188, [M�H-H2O]at m/z 352 and [M�H-2CH3O-OH]at m/z 290, which was tentatively identified as -allocryptopine [10,14].Methyl 4-bromo-5-methoxypicolinate Data Sheet The MS/MS data of compound five revealed its most important fragmentation, which was the successive losses of CH3, C10H12O2, C11H15O2, C11H14O2N, yielding solution ions at m/z 354, 206, 192 and 165, corresponding for the structure of corydaline [15,16].PMID:23557924 Compound 35 made [M�H]ion at m/z 340, fragment ions [M�H-C10H12O2]at m/z 176 and [M�H-CH3-C10H10O2N]at m/z 149. Therefore, it may be identified as tetrahydroberberine [10]. Four compounds had the same [M�H]ions at m/z 356 (compounds two, 21, 28, and 30). Compound two, 28 and 30 all created fragment ion [M�H-C10O2H12]at m/z 192, which resulted in the RDA rupture of tetrahydroprotoberberine alkaloids [14]. Compound 28 was confirmed as tetrahydropalmatine after comparing with a reference normal and literature [14,16]. Compound 30 had the identical characteristic fragmentation pathway, but its retention time was distinctive from that of tetrahydropalmatine. Consequently, it was tentatively identified as rotundine. Compound two was tentatively identified as yuanhunineAnalysis of common peaks in chemical fingerprint of YZTTableRecovery of each and every analyte determined by standard addition approach (n3).Original quantity (g) Spiked amount (g) Discovered amount (g) Recovery ( ) Typical recovery ( ) RSD ( ) 93.53 46.77 93.53 140.00 3.40 6.80 ten.00 37.50 74.00 112.00 52.62 105.00 157.62 27.75 55.50 83.00 2.32 four.70 7.00 24.42 50.00 74.42 93.38 187.00 280.00 39.92 80.00 120.00 46.53 93.00 140.00 139.46 190.80 239.13 9.99 14.00 17.00 112.76 152.58 191.12 156.82 207.78 259.05 82.98 112.27 140.61 6.89 9.28 11.73.