Simultaneous determination of synephrine, arecoline, and norisoboldine in Chinese patent medicine Si-Mo-Tang oral liquid preparation by strong cation exchange high performance liquid chromatography

Figures & data

Table 1.  Chromatographic parameters of resolution, theoretical plate number, symmetry factor, and peak purity of arecoline, synephrine, and norisoboldine in SMT on SCX and ZORBAX SB-C18 columns.

Parameters		Synephrine		Norisoboldine		Arecoline
		SCX	ZORBAX SB-C18	SCX	ZORBAX SB-C18	SCX	ZORBAX SB-C18
Resolution		4.57	1.04	1.67	14.49	8.47	2.37
Number of theoretical plates		11781	9890	9084	13994	11672	4200
Symmetry factor		0.92	0.68	0.86	0.69	0.91	0.61
Peak Purity	Purity factor	999.885	810.509	999.892	794.063	999.799	636.696
	Threshold limit	999.639	997.612	999.789	997.944	999.442	996.321

Figure 1.  Structures of arecoline, synephrine, and norisoboldine.

Figure 2.  HPLC chromatograms of reference standards (A) and SMT sample (B) separated on an Agilent ZORBAX SB-C18 column (250 × 4.6 mm, 5 µm) (1: synephrine; 2: arecoline; 3: norisoboldine).

Figure 3.  HPLC chromatograms of reference standards (A) and SMT sample (B) separated on an Agilent SCX column (250 × 4.6 mm, 5 µm) (1: synephrine; 2: norisoboldine; 3: arecoline).

Table 2.  Accuracy and recovery of synephrine, arecoline and norisoboldine at different concentrations (n = 3).

Compounds	Background amount (mg)	Added amount (mg)	Observed amount (mg)	RSD (%)	Accuracy (Relative error, %)	Recovery (%)	Average recovery (%)	RSD (%)
Synephrine	0.0559	0.0255	0.0821	0.84	−3.53	96.30
		0.0510	0.1081	0.61	−0.78	99.14	98.99	2.64
		0.0612	0.1196	1.27	1.47	101.52
Arecoline	0.0879	0.0821	0.1674	0.64	−3.29	96.65
		0.1027	0.1862	0.12	−4.38	95.63	95.63	1.07
		0.1283	0.2098	0.05	−5.38	94.60
		0.0605	0.1587	0.39	−0.50	99.55
Norisoboldine	0.0985	0.0968	0.1927	0.59	−2.69	97.36	99.04	1.51
		0.1210	0.2197	0.14	0.16	100.22

Table 3.  Determination of synephrine, arecoline and norisoboldine from 26 batches of SMT (n = 3).

No.	Batch	Manufacturer*	Content (mg mL^−1) (mean ± SD)**
			Synephrine	Norisoboldine	Arecoline
1	070109	A	0.021	0.021	0.026
2	070419	A	0.024	0.024	0.036
3	070706	A	0.031	0.042	0.024
4	071017	A	0.022	0.028	0.022
5	080121	A	0.021	0.036	0.026
6	080421	A	0.018	0.040	0.023
7	080712	A	0.022	0.041	0.025
8	081036	A	0.027	0.038	0.027
9	090225/731	A	0.027	0.044	0.030
10	090628/477	A	0.027	0.056	0.043
11	091026/470	A	0.034	0.054	0.035
12	091243/448	A	0.040	0.049	0.037
13	090424	A	0.024	0.044	0.021
14	090425	A	0.025	0.046	0.033
15	090426	A	0.024	0.046	0.028
16	090435	A	0.027	0.046	0.042
17	090436	A	0.022	0.039	0.035
18	20060311	A	0.020	0.040	0.023
19	20060601	B	0.015	0.042	0.036
20	20060905	B	0.019	0.046	0.037
21	20061203	B	0.022	0.042	0.029
22	20070308	B	0.022	0.039	0.026
23	20070624	B	0.028	0.043	0.019
24	20070918	B	0.021	0.021	0.028
25	20071201	B	0.019	0.042	0.022
26	20080306	B	0.026	0.043	0.028

*A: Hunan Hansen Pharmaceutical Co., Ltd. Hunan; B: Hunan Zhongda Wuma Pharmaceutical Co., Ltd.

**The standard deviation (SD) values for all data were smaller than 0.002.