中空纤维液相微萃取-高效液相色谱法测定荆芥及其复方制剂中胡薄荷酮的含量
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篇名: 中空纤维液相微萃取-高效液相色谱法测定荆芥及其复方制剂中胡薄荷酮的含量
TITLE: Content Determination of Pulegone in Schizonepeta tenuifolia and Its Compound Preparation by Hollow Fiber Liquid-phase Microextraction Coupled with HPLC
摘要: 目的:建立荆芥饮片及其复方制剂中胡薄荷酮的含量测定方法。方法:采用中空纤维液相微萃取-高效液相色谱法(HF-LPME-HPLC)。在单因素实验基础上,以胡薄荷酮富集倍数为考察指标,样品相溶液盐(NaCl)浓度、萃取时间、搅拌速度为考察因素,采用中心组合设计-响应面法优化荆芥饮片及其复方制剂(以复方荆芥颗粒为例)的HF-LPME条件,并进行验证。采用HPLC法测定胡薄荷酮的含量,色谱柱为HypersilC18,流动相为甲醇-0.3%磷酸溶液(梯度洗脱),流速为1.0mL/min,检测波长为252nm,柱温为25℃,进样量为20μL。以2020年版《中国药典》(一部)荆芥饮片项下HPLC法为参照,验证本研究所建HF-LPME-HPLC法的可行性。结果:HF-LPME最优条件为以正壬醇为萃取溶剂,在pH为7、NaCl浓度为11%的样品相溶液中,以800r/min搅拌萃取36min。HPLC方法学考察结果显示,胡薄荷酮检测质量浓度的线性范围为0.05~5μg/mL(r=0.9990);检测限和定量限分别为0.4、1.3ng/mL;日内、日间精密度的RSD分别为1.8%~4.0%、1.5%~4.1%(n=3);重复性、稳定性(24h)试验的RSD均小于8%(n=6);荆芥饮片和复方荆芥颗粒中胡薄荷酮的平均回收率分别为102.6%~105.1%、97.2%~102.3%,RSD分别不高于4.1%和6.2%(n=3)。采用药典方法和本研究建立方法测得荆芥饮片中胡薄荷酮的平均含量分别为0.84mg/g(RSD=4.3%,n=3)和0.87mg/g(RSD=5.5%,n=3),差异无统计学意义(P>0.05)。结论:建立的HF-LPME-HPLC法实现了对胡薄荷酮的富集与浓缩,具有较强的纯化能力与较高的灵敏度,可用于荆芥饮片及其复方制剂中胡薄荷酮的含量测定。
ABSTRACT: OBJECTIVE:To establish t he metho d for the content determination of pulegone in Schizonepetae tenuifolia decoction pieces and its compound preparation. METHODS :Hollow fiber liquid-phase microextraction coupled with HPLC (HF-LPME-HPLC) was adopted. Based on single factor tests ,HF-LPME condition of S. tenuifolia decoction pieces and its compound preparation (taking Compound S. tenuifolia granule as an expample ) was optimized by central composite design-response surface methodology using pulegone enrichment multiple as index ,with the concentration of sample phase solution (NaCl),extraction time and stirring speed as factors. Validation test was conducted. HPLC method was adopted to determine the content of pulegone. The determination was performed on Hypersil C 18 column with mobile phase consisted of methanol- 0.3% phosphoric acid (gradient elution )at the flow rate of 1.0 mL/min. The detection wavelength was set at 252 nm,the column temperature was 25 ℃. The sample size was 20 μL. The feasibility of HF-LPME-HPLC method established in this study was validated by using HPLC method stated in the item of S. tenuifolia decoction pieces in 2020 edition of Chinese Pharmacopoeia (part Ⅰ)as reference. RESULTS :The optimum HF-LPME conditions included n-nonanol as the extraction solvent ,sample phase solution with 11% NaCl and pH value of 7,stirring speed of 800 r/min,extraction time of 36 min. Results of HPLC methodology investigation showed that linear range of pulegone were 0.05-5 μg/mL(r=0.999 0). The limits of detection and quantitation were 0.4 and 1.3 ng/mL,respectively. RSDs of intra-day and inter-day precision were 1.8%-4.0% and 1.5%-4.1%(n=3),respectively. RSDs of reproducibility and stability tests (24 h)were all lower than 8%(n=6). Average recoveries of S. tenuifolia decoction pieces and Compound S. tenuifolia granule were 102.6%-105.1% and 97.2%-102.3%,respectively;RSDs were not higher than 4.1% and 6.2%(n=3). The average contents of pulegone in S. tenuifolia decoction pieces determined by pharmacopoeia method and established method were 0.84 mg/g(RSD=4.3% ,n=3)and 0.87 mg/g(RSD=5.5% ,n=3),respectively,with no significant difference (P>0.05). CONCLUSIONS :The established HF-LPME-HPLC method can enrich and concentrate pulegone , shows strong purification ability and high sensitivity ,and can be used to determine the contents of pulegone in S. tenuifolia decoction pieces and its compound preparation.
期刊: 2021年第32卷第12期
作者: 李萍,胡爽,白小红,毕小平
AUTHORS: LI Ping,HU Shuang ,BAI Xiaohong ,BI Xiaoping
关键字: 中空纤维液相微萃取;高效液相色谱法;中心组合设计-响应面法;胡薄荷酮;荆芥饮片;复方制剂
KEYWORDS: Hollow fiber liquid-phase microextraction ;HPLC;Central composite design-response surface methodology ;
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