Schisandra Quality Control Methods

High performance liquid and Gas chromatographic fingerprint chromatogram were established for Schisandra chinensis(Turcz.)Baill.and Schisandra sphenanthera Rehd.et Wils.And Quality assessment and identification was researched for Schisandra chinensis (Turcz.)Baill.and Schisandra sphenanthera Rehd.et Wils.Simultaneous determination of 4 compounds in Volatile Fractions of Schisandra chinensis(Turcz.)Baill.,the methods of Quantitative Determination of 10 Lignans Constituents from Schisandra chinensis.Baill.by HPLC,and Quantitative Determination of 3 kinds of fatty acids from Schisandra chinensis. Baill.by GC were respectively established.It was systemic that the methods of quality control of Schisandra chinensis(Turcz.)Baill.and Schisandra sphenanthera Rehd.et Wils.was researched.The methods above provided reliable basis to distinguish Schisandra chinensis (Turcz,)Baill.and Schisandra sphenanthera Rehd.et Wils.,as well as references to use Schisandra chinensis(Turcz.)Baill.and Schisandra sphenanthera Rehd.et Wils.reasonably.We established a method of Gas chromatographic fingerprint chromatogram for Schisandra chinensis(Turcz.)Baill.and Schisandra sphenanthera Rehd.et Wils.capillary column DB-17(30 m×0.25 mm×0.25μm)was used.The detector was FID.Inlet temperature was 230℃.The detector temperature was 250℃.Column temperature:50℃(2 min)(?)130℃(20 min)(?)190℃(6 min)(?)210℃(3 min). Carrying gas was nitrogen(1.2 mL·min^-1).Split ratio was 50:1.Volume was 1μL.14 batches of Schisandra chinensis(Turcz.)Baill.and 12 batches of Schisandra sphenanthera Rehd.et Wils was determined by GC.The hierarchical cluster was applied to the fingerprints of 14 batches of Schisandra chinensis(Turcz.)Baill.and 12 batches of Schisandra sphenanthera Rehd.et Wils.The 14 batches of Schisandra chinensis(Turcz.)Baill.was divided into two grades.Among them the gradeâ… was commendatory,and the gradeâ…¡was general.Mutual pattern was established from 12 batches in the gradeâ… by using the fingerprint chromatogram software required to use by the Chinese Pharmacopoeia Committee.Similarity calculations were studied by comparing the GC fingerprint chromatograms of Schisandra chinensis (Turcz.)Baill.and mutual pattern.The 12 batches of Schisandra sphenanthera Rehd.et Wils. was divided into two grades.Among them the gradeâ… was commendatory and the gradeâ…¡ was general.Mutual pattern was established from 11 batches in the gradeâ… by using the fingerprint chromatogram software required to use by the Chinese Pharmacopoeia Committee. Similarity calculations were studied by comparing the GC fingerprint chromatograms of Schisandra sphenanthera Rehd.et Wils.And the result of the commendatory should be all over 0.90 and the other samples were the general.GC fingerprint chromatograms were applied to identify Schisandra chinensis(Turcz.)Baill.and Schisandra sphenanthera Rehd.et Wils.We established a method of high performance liquid chromatographic fingerprint chromatogram for Schisandra chinensis(Turcz.)Baill.The separation was performed on a Luna C₁₈analytical column(250 mm×4.6 mm,5μm)with the mobile phase consisting of water and acetonitrile with gradient elution mode at the flow rate of 0.8 mL·min^-1.Elution procedure:0～20 min,45%B～65%B;20～26 min,65%B;26～50 min,75%B.The detection was set at 220 nm.14 batches of Schisandra chinensis(Turcz.)Baill.was determined by HPLC fingerprint chromatogram.The Hierarchical cluster was applied to the fingerprints of 14 batches of Schisandra chinensis(Turcz.)Baill.And the 14 batches of Schisandra chinensis(Turcz.)Baill.was divided into two grades.Among them the gradeâ… was commendatory and the gradeâ…¡was general.Mutual pattern was established from 13 batches in the gradeâ… by using the fingerprint chromatogram software required to use by the Chinese Pharmacopoeia Committee.Similarity calculations were studied by comparing the GC fingerprint chromatograms of Schisandra chinensis(Turcz.)Baill.and mutual pattern,the result of the commendatory should be all over 0.90 and the other samples were the general.We established the method of simultaneous determination of 4 compounds in Volatile Fractions of Schisandra chinensis(Turcz.)Balll.Capillary column DB-17(30 m×0.25 mm×0.25μm)was used.The detector was FID.Inlet temperature was 230℃.The detector temperature was 250℃.Column temperature:50℃(2 min)(?)130℃(5 min). Carrying gas was nitrogen(1.2 mL·min^-1).Split ratio was 10:1.Volume was 1μL.GC method was applied for the determination ofα-pinene,β-pinene,limonene and bornyl acetate from the essential oil.The linear ranges forα-pinene,β-pinene,limonene and Bornyl acetate were 0.020～0.205 mg·mL(-1)(r = 0.9998),0.006～0.104 mg·mL^-1(r = 0.9993),0.006～0.162 mg·mL^-1(r = 0.9994)and 0.040～1.000 mg·mL^-1(r = 0.9993).The mean recoveries were 100.8%(RSD = 1.1%),98.7%(RSD = 2.9%),99.4%(RSD = 0.9%)and 96.4%(RSD = 0.4%),respectively.We established the method of quantitative Determination of 10 Lignans Constituents from Schisandra chinensis.Baill.by HPLC.The separation was performed on a Luna C₁₈ analytical column(250 mm×4.6 mm,5μm)with the mobile phase consisting of water and acetonitrile with gradient elution mode at the flow rate of 0.8 mL·min^-1.Elution procedure:0～20 min,45%B～65%B;20～26 min,65%B;26～50 min,75%B.The detection was set at 220 nm.The HPLC method described in this paper used photodiode array detection to determine the lignans,Schizandrin(Schi),Gomisin-D(G-D),Gomisin-J(G-J),Aomisin (Aom),Pregomisin(Preg),Angeloygomisin-H(Ange-H),Tigloylgomisin-P(Tig-P), Deoxyschisandrin(Deo-schi),Gomisin N(G-N)andγ-schisandrin(γ-schi)in the fruits of S. chinensis.The linear ranges for these were 20～200μg·mL^-1(γ= 0.9999),2～20μg·mL^-1(r = 0.9998),4～40μg·mL^-1(r= 0.9999),13.3～133.3μg.mL^-1(r = 0.9999),4～40μg·mL^-1(r = 0.9995),6.25～62.5μg·mL^-1(r = 0.9999),6.67～66.7μg·mL^-1(r = 1.0000),4～40μg·mL^-1 (r = 0.9999),4～40μg·mL^-1(r = 0.9997)and 10～100μg·mL^-1(r = 1.0000).The mean recoveries were 99.3%(RSD = 2.5%),100.2%(RSD = 2.5%),102.1%(RSD = 1.6%),98.5% (RSD = 2.4%),96.5%(RSD = 3.2%),99.4%(RSD = 2.8%),99.1%(RSD = 2.7%),97.5% (RSD = 2.5%),101.9%(RSD = 3.1%)and 100.6%(RSD = 3.5%).We established the method of quantitative Determination of 3 kinds of fatty acids from Schisandra chinensis.Baill.by GC.Capillary column DB-17(30 m×0.25 mm×0.25μm) was used.The detector was FID.Inlet temperature was 250℃.The detector temperature was 250℃.Column temperature:150℃(2 min)(?)250℃.Carrying gas was nitrogen(1.2 mL·min^-1),split ratio was 10:1.Volume was 1μL.GC method was applied for the determination of palmitic acid,oleic acid and linoleic acid.The linear ranges for palmitic acid, oleic acid and linoleic acid were 0.01～0.1 mg·mL^-1(r = 0.9997),0.038～0.380 mg·mL^-1(r = 0.9997)and 0.215～2.15 mg·mL^-1(r = 0.9992).The mean recoveries were 99.4%(RSD = 2.4%),96.3%(RSD = 2.4%)and 96.4%(RSD = 2.1%).