Rapid simultaneous identification and determination of the multiple compounds in crude Fructus Corni and its processed products by HPLC–MS/MS with multiple reaction monitoring mode

Figures & data

Figure 1.  The chemical structures of the eight bioactive compounds in Fructus Corni.

Table 1.  MS/MS detection parameters for the eight bioactive compounds in Fructus Corni.

Compound	Precursor ion (m/z)	Product ion	Dwell time (ms)	Fragmentation (V)	Collision energy (eV)
Gallic acid	169	125	750	100	10
		97			17
5-HMF	127	109	750	80	5
		81			10
Morroniside	451	243	750	100	12
		179			15
Sweroside	403	179	175	100	20
		125			20
Cornin	433	225	175	100	5
		101			20
Loganin	435	389	175	100	10
		227			10
7-O-Methyl-morroniside	465	397	175	100	20
		257			8
Cornuside	541	347	750	180	22
		169			30

Table 2.  Summary of regression data, LOD, LOQ for the eight bioactive compounds in Fructus Corni.

Analyte	Calibration curve	R^2	Linear range (ng/mL)	LOD (ng/mL)	LOQ (ng/mL)
Gallic acid	Y = 154.1525X + 4450.62	0.9977	15.87–3174	0.4232	1.2692
5-HMF	Y = 315.6922X + 123634.84	0.9922	65–13100	0.0042	0.0419
Morroniside	Y = 42.1687X − 4703.985	0.9934	37.5–7500	1.2000	6.0000
Sweroside	Y = 10.3480X − 127.292	0.9948	5.325–1065	3.6210	13.8450
Cornin	Y = 37.2123X − 849.629	0.9962	9.375–1875	0.2976	0.5952
Loganin	Y = 18.9672X − 1522.261	0.9957	25.125–5025	10.5600	31.6800
7-O-Methyl-morroniside	Y = 14.6983X − 172.229	0.9963	5.115–1023	12.7875	34.1000
Cornuside	Y = 251.3523X + 658.36	0.9989	5.25–1050	1.4000	3.3250

Figure 2.  The LC-MS/MS chromatographic profiles of Fructus Corni samples. 1: gallic acid; 2: 5-HMF; 3: morroniside; 4: sweroside; 5: cornin; 6: loganin; 7: 7-O-methyl-morroniside; 8: cornuside.

Table 3.  The mean contents of the eight bioactive compounds in crude and processed Fructus Corni samples (mg/g + SD, n = 5).

Sample	Gallic acid	5-HMF	Morroniside	Sweroside	Cornin	Loganin	7-O-Methyl-morroniside	Cornuside
Crude 1	0.9495 ± 0.0205	–	3.6421 ± 0.0641	0.4925 ± 0.0118	0.1458 ± 0.0015	3.4607 ± 0.0737	0.0604 ± 0.0014	1.4351 ± 0.0342
Crude 2	0.9578 ± 0.0207	–	3.9725 ± 0.0699	0.4987 ± 0.0119	0.1654 ± 0.0017	3.4168 ± 0.0728	0.0582 ± 0.0014	1.5975 ± 0.0380
Crude 3	0.9360 ± 0.0202	–	5.1757 ± 0.0911	0.4713 ± 0.0113	0.1878 ± 0.0020	4.1066 ± 0.0875	0.0547 ± 0.0013	1.5943 ± 0.0379
JZP 1	2.1357 ± 0.0461	5.7855 ± 0.1406	3.4335 ± 0.0604	0.5495 ± 0.0131	0.1904 ± 0.0020	3.4847 ± 0.0742	0.0880 ± 0.0021	0.9803 ± 0.0233
JZP 2	2.3139 ± 0.0500	6.9377 ± 0.1686	3.6426 ± 0.0641	0.5664 ± 0.0135	0.1963 ± 0.0020	3.5484 ± 0.0756	0.1005 ± 0.0024	1.1349 ± 0.0270
JZP 3	2.2658 ± 0.0489	7.7759 ± 0.1890	3.1186 ± 0.0549	0.4922 ± 0.0118	0.1895 ± 0.0020	4.0011 ± 0.0852	0.0976 ± 0.0023	1.2075 ± 0.0287

Figure 3.  The mass spectra of the eight bioactive compounds. Each compound was collected from HPLC and analyzed by mass spectra.