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Objective To study the method of headspace gas chromatography for the determination of β-eugenol in Magnolia officinalis. Methods Headspace gas chromatography was used. The column was HP-INNOWax capillary column, the detector was hydrogen flame ionization detector, inlet temperature: 200 ℃; column temperature: 135 ℃ for 3min, at 10 ℃/min heating rate rose to 150 ℃, At a rate of 15 ℃/min up to 250 ℃for 5 min; constant flow rate: 0.8 mL/min; detector temperature: 250 ℃; headspace injection, gas injection volume: 1 mL, headspace Temperature 180 ℃, the balance time 30min; with the external standard method according to the peak area calculation results. Results The linear range of the concentration of menthol was 2.49～24.86 μg/mL (r=0.9994). The RSD of the precision, stability and repeatability test were <5％, the average recovery was 97.0％, RSD was 0.84％ (n=9). Conclusion The method is simple and accurate for the determination of volatile oil.
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OBJECTIVE:To provide reference for improving the quality of Gelatin hollow capsule. METHODS:Atomic fluo-rescence spectrometry was used to determine the contents of Hg,As in Gelatin hollow capsule;graphite furnace atomic absorption spectrometry was used to determine the contents of Cr,Pb,Cd;flame atomic absorption spectrometry was used to determine the contents of Cu,Zn;and the contents of 7 elements in 48 batches of commercially available Gelatin hollow capsule were deter-mined. RESULTS:Each element showed good linear relationship in each mass concentration range(Cr,Pb,Cd,As and Hg were respectively 0-10,0-20,0-1.5,0-10,0-1.0μg/L;Cu and Zn were 0-1.8 mg/L)(r≥0.9969). The detection limits of Cr,Pb,Cd, Cu,Zn,Hg and As were 0.065,0.007,0.011,0.004,0.010,0.108,0.004 μg/L,respectively. RSDs of precision tests were no more than 2.5%(n=6);RSDs of reproducibility tests were no more than 7.5%(n=6);average recoveries ranged in 88.6%-109.5%(RSD≤6.7%,n=6). The contents of 7 elements in the 48 batches of samples were in line with the relevant provi-sions in Chinese Pharmacopoeia(2015 edition,part 4)and pharmacopoeia or standards in other countries or organizations. CON-CLUSIONS:The method shows high sensitivity,high precision with accurate and reliable results,and can be used for the content determination of Cr,Pb,Cd,Cu,Zn,Hg and As in Gelatin hollow capsule. The 48 batches of Gelatin hollow capsule from differ-ent manufacturers have good quality.
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OBJECTIVE:To provide reference for improving the quality of Gelatin hollow capsule. METHODS:Atomic fluo-rescence spectrometry was used to determine the contents of Hg,As in Gelatin hollow capsule;graphite furnace atomic absorption spectrometry was used to determine the contents of Cr,Pb,Cd;flame atomic absorption spectrometry was used to determine the contents of Cu,Zn;and the contents of 7 elements in 48 batches of commercially available Gelatin hollow capsule were deter-mined. RESULTS:Each element showed good linear relationship in each mass concentration range(Cr,Pb,Cd,As and Hg were respectively 0-10,0-20,0-1.5,0-10,0-1.0μg/L;Cu and Zn were 0-1.8 mg/L)(r≥0.9969). The detection limits of Cr,Pb,Cd, Cu,Zn,Hg and As were 0.065,0.007,0.011,0.004,0.010,0.108,0.004 μg/L,respectively. RSDs of precision tests were no more than 2.5%(n=6);RSDs of reproducibility tests were no more than 7.5%(n=6);average recoveries ranged in 88.6%-109.5%(RSD≤6.7%,n=6). The contents of 7 elements in the 48 batches of samples were in line with the relevant provi-sions in Chinese Pharmacopoeia(2015 edition,part 4)and pharmacopoeia or standards in other countries or organizations. CON-CLUSIONS:The method shows high sensitivity,high precision with accurate and reliable results,and can be used for the content determination of Cr,Pb,Cd,Cu,Zn,Hg and As in Gelatin hollow capsule. The 48 batches of Gelatin hollow capsule from differ-ent manufacturers have good quality.
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OBJECTIVE:To establish a method for the content determination of menthanol in Qinagli pipa syrup. METHODS:Headspace GC was performed on the column of HP-INNOWax capillary column,column temperature was 80 ℃,temperature inlet sample was 150 ℃,the detector was hydrogen flame ionization detector with temperature of 250 ℃,the flow rate of nitrogen was 0.8 ml/min with constant flow and no split,the volume injection was 1 ml,the equilibrium temperature of headspace bottle was 80 ℃,and the equilibrium time was 20 min. RESULTS:The linear range of menthanol was 2.486-24.86 μg/ml(r=0.9999),RS-Ds of precision,stability and reproducibility tests were lower than 2%,recovery was 95.4%-99.8%(RSD=1.5%,n=9). CON-CLUSIONS:The method is simple and accurate,and can be used for the content determination of menthanol in Qinagli pipa syrup.
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Objective:To determine the contents of 5 heavy mental elements , Cr, Pb, Cd, Cu and Zn, in vacant gelatin capsule shells.Methods:Graphite furnace atomic absorption spectrometry was used to determine Cr , Pb and Cd, and flame atomic absorption spectrometry was used to determine Cu and Zn .Results: The vacant gelatin capsule shells contained Cr , Pb, Cd, Cu and Zn up to 1.850, 0.404, 0.019, 6.295,5.839 mg· kg-1, respectively.Conclusion:The method can be used for the content determination of Cr, Pb, Cd, Cu and Zn in vacant gelatin capsule shells , which provides scientific basis for the development of quality standard .
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Objective:To establish an HPLC method for the simultaneous determination of hesperidin and phillyrin in Siji Gamao capsules. Methods:HPLC was applied with the chromatographic conditions as follows:the chromatographic column was Agilent-XDB C18 (250 mm × 4. 6 mm,5μm) at 30℃, the mobile phase was methanol-0. 1% phosphoric acid solution with gradient elution, the flow rate was 1. 0 ml·min-1 , the detection wavelength was 277nm and the injection volume was 5μl. Results:The linear range of hesperi-din and phillyrin was 12.000-60.000 μg·ml-1(r=0.999 6) and 18.000-90.000 μg·ml-1(r=0.999 3),respectively; the average recovery was 96.61%(RSD=1.40%) and 97.66%(RSD=1.27%), respectively. Conclusion: The method is simple, accurate and repeatable, which can be used in the quality control of Siji Ganmao capsules.