分散固相萃取-高效液相色谱-串联质谱法同时测定保健品片剂中5种黄芩素类化合物

doi:10.3724/SP.J.1123.2019.11008

摘要/Abstract

摘要：

基于分散固相萃取-高效液相色谱-串联质谱技术（DSPE-HPLC-MS/MS），建立了同时测定保健品片剂中野黄芩素、4'-羟基汉黄芩素、去甲汉黄芩素、黄芩素和汉黄芩素的分析方法。以10 mL丙酮提取保健品片剂中的目标成分，75 mg C₁₈吸附剂进行净化。通过优化提取溶剂、吸附剂的种类和用量，达到了提取和净化的目的。结果表明，5种目标物在各自的线性范围内具有良好的线性关系，相关系数（r）均大于0.99，检出限为0.5~40 μg/kg，定量限为2.0~120 μg/kg。使用3种保健品片剂基质进行定量限的1倍、5倍、10倍3个添加水平的加标回收试验，5个目标物的平均回收率为83.1%~106.5%，精密度为0.97%~4.52%。该方法操作简单、灵敏度高、重现性好，适用于保健品片剂中黄芩素类化合物的同时测定。

关键词: 分散固相萃取, 高效液相色谱-串联质谱法, 黄芩素, 保健品

Abstract:

A method based on dispersive solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry (DSPE-HPLC-MS/MS) was developed for the simultaneous determination of five analytes scutellarein, 4'-hydroxywogonin, norwogonin, baicalein, and wogonin in healthy product tablets. The samples were extracted with 10 mL acetone and purified on 75 mg C₁₈. The types and dosages of the extracted solvents and adsorbents were optimized. The results showed that these five analytes exhibited good linear relationships in their respective linear ranges. The correlation coefficients (r) were more than 0.99. The detection limits and quantitative limits were 0.5-40 μg/kg and 2.0-120 μg/kg, respectively. Recovery tests were carried out using three kinds of health product tablet matrices. The concentrations were one, five, and ten times the quantitative limit. The average recovery of these five targets was 83.1% to 106.5%, with relative standard deviations (RSDs) ranging from 0.97% to 4.52%. This method is easy to operate, and it shows high sensitivity and good reproducibility. Thus, it is suitable for the simultaneous determination of the target compounds in health tablets.

Key words: dispersive solid-phase extraction (DSPE), high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), baicalein, health product

岑建斌, 梁志森, 区硕俊, 黄嘉乐, 李秀英, 林青兰, 陈玉珍, 刘炘杰, 林森煜. 分散固相萃取-高效液相色谱-串联质谱法同时测定保健品片剂中5种黄芩素类化合物[J]. 色谱, 2020, 38(6): 672-678.

CEN Jianbin, LIANG Zhisen, OU Shuojun, HUANG Jiale, LI Xiuying, LIN Qinglan, CHEN Yuzhen, LIU Xinjie, LIN Senyu. Simultaneous determination of five baicaleins in healthy product tablets by dispersive solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(6): 672-678.

图/表 10

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Compound	Retention time/min	Ionization model	Precursor ion (m/z)	Product ion (m/z)	Collision energy/eV	RF lens/V
* Quantitative ion.
Scutellarein	10.1	ESI⁺	287.0	123.0^*	32.6	135.9
				169.1	29.2	135.9
4′-Hydroxywogonin	12.0	ESI⁺	301.1	286.0^*	23.1	139.0
				195.1	36.2	139.0
Norwogonin	12.4	ESI⁺	271.1	169.0^*	29.4	149.0
				115.1	45.6	149.0
Baicalein	12.7	ESI⁺	271.1	123.0^*	31.5	141.0
				253.0	24.3	141.0
Wogonin	14.4	ESI⁺	285.1	270.0^*	22.5	126.8
				151.1	44.0	126.8

Compound	Retention time/min	Ionization model	Precursor ion (m/z)	Product ion (m/z)	Collision energy/eV	RF lens/V
* Quantitative ion.
Scutellarein	10.1	ESI⁺	287.0	123.0^*	32.6	135.9
				169.1	29.2	135.9
4′-Hydroxywogonin	12.0	ESI⁺	301.1	286.0^*	23.1	139.0
				195.1	36.2	139.0
Norwogonin	12.4	ESI⁺	271.1	169.0^*	29.4	149.0
				115.1	45.6	149.0
Baicalein	12.7	ESI⁺	271.1	123.0^*	31.5	141.0
				253.0	24.3	141.0
Wogonin	14.4	ESI⁺	285.1	270.0^*	22.5	126.8
				151.1	44.0	126.8

Compound	Average recoveries/%
	GCB/mg			PSA/mg			C₁₈/mg
	10	25	50	10	25	50	10	25	50	75	100	125
Scutellarein	0.00	0.00	0.00	0.00	0.00	0.00	95.9	95.3	95.5	97.4	46.5	46.5
4′-Hydroxywogonin	1.67	1.52	0.321	32.3	11.1	3.50	104	103	103	104	98.7	98.7
Norwogonin	0.00	0.00	0.00	0.00	0.00	0.00	101	100	101	101	83.3	82.7
Baicalein	0.00	0.00	0.00	0.00	0.00	0.00	85.9	85.1	85.4	87.5	62.7	63.2
Wogonin	2.86	1.84	0.680	91.4	88.3	78.3	98.5	100	99.7	101	97.5	99.1

Compound	Average recoveries/%
	GCB/mg			PSA/mg			C₁₈/mg
	10	25	50	10	25	50	10	25	50	75	100	125
Scutellarein	0.00	0.00	0.00	0.00	0.00	0.00	95.9	95.3	95.5	97.4	46.5	46.5
4′-Hydroxywogonin	1.67	1.52	0.321	32.3	11.1	3.50	104	103	103	104	98.7	98.7
Norwogonin	0.00	0.00	0.00	0.00	0.00	0.00	101	100	101	101	83.3	82.7
Baicalein	0.00	0.00	0.00	0.00	0.00	0.00	85.9	85.1	85.4	87.5	62.7	63.2
Wogonin	2.86	1.84	0.680	91.4	88.3	78.3	98.5	100	99.7	101	97.5	99.1

Compound	K values
Compound	Sea cucumber oyster health tablet	Tabletting candy	Vitamin tablet
Scutellarein	1.19	0.86	0.83
4′-Hydroxywogonin	0.47	1.76	9.07
Norwogonin	2.70	2.27	2.24
Baicalein	1.19	1.14	1.11
Wogonin	1.20	3.28	0.86