Yu Bingsheng, Sheng Dongdi, Tan Qiumin
Chemistry and Chemical Engineering School, Lingnan Normal University.
Chem Pharm Bull (Tokyo). 2019 Jul 1;67(7):713-716. doi: 10.1248/cpb.c18-00968. Epub 2019 Apr 19.
A reverse phase (RP)-HPLC method for separation and determination of Schisandrin A and Schisandrin B was presented, using a C18 Bondclone column, with methanol-water (v/v = 68 : 32) as mobile phase at a flow-rate of 1.00 mL·min, and UV detection at 220 nm. The tested parameters included mobile phase composition and UV detection wavelength. Good linearities were observed within concentration ranges of Schisandrin A 0.008-4.8 mg·L (r = 0.9996), and Schisandrin B 0.005-3.1 mg·L (r = 0.9994), respectively. The limit of detection (LOD) (S/N = 3) were 0.005 mg·L Schisandrin A and 0.002 mg·L Schisandrin B, respectively. The method was applied to determine the 2 compounds in a traditional Chinese medicine preparation for treatment of hepatic diseases, Huganpian tablet. To eliminate matrix effect, Oasis hydrophilic lipophilic balance (HLB) solid-phase extraction (SPE) was used to purify the ultra-sonicately extracted solution of the drug sample. Combined with the HLB SPE purification procedure, the HPLC method gave satisfactory results for quantitation of Schisandrin A and Schisandrin B in 3 types of Huganpian tablet samples, with spiking recoveries ca. 98% (relative standard deviation (R.S.D.) ≤ 3.5%) (n = 5).
建立了一种反相（RP）-高效液相色谱法用于五味子醇甲和五味子乙素的分离与测定，采用C18 Bondclone色谱柱，以甲醇-水（体积比为68∶32）为流动相，流速为1.00 mL·min，在220 nm波长处进行紫外检测。所考察的参数包括流动相组成和紫外检测波长。在五味子醇甲浓度范围为0.008～4.8 mg·L（r = 0.9996）和五味子乙素浓度范围为0.005～3.1 mg·L（r = 0.9994）内均呈现良好的线性关系。检测限（S/N = 3）分别为五味子醇甲0.005 mg·L和五味子乙素0.002 mg·L。该方法应用于测定一种治疗肝病的中药制剂护肝片中的这2种化合物。为消除基质效应，采用Oasis亲水亲脂平衡（HLB）固相萃取（SPE）法对药物样品的超声提取液进行净化。结合HLB SPE净化程序，该高效液相色谱法对3种护肝片样品中五味子醇甲和五味子乙素的定量分析结果令人满意，加样回收率约为98%（相对标准偏差（R.S.D.）≤3.5%）（n = 5）。
