ABSTRACT
OBJECTIVE：To establish the m ethod for the simultaneous determination of 6 carbohydrate related substances in glucose as fructose ，maltose，isomaltose，maltotriose，maltotetraose and maltopentaose. METHODS ：HPLC-ELSD was adopted. The determine was performed on XBridge Amide column with mobile phase consisted of acetonitrile-water （75∶25，V/V）at a flow rate of 0.5 mL/min. The column temperature was set at 30 ℃，and the sample size was 10 L. The detector was evaporative light scattering detector ，the carrier gas was nitrogen ，the gas pressure was 40 psi，the evaporation temperature was 80 ℃，the drift tube temperature was 80 ℃，and the gain was 100. RESULTS ：The linear range of 6 carbohydrate related substances were 5.99-59.88， 9.90-98.96，9.92-99.19，5.97-59.74，4.03-40.32，5.89-58.89 μg/mL（r＞0.999 0）. The quantitation limits were 1.5，1.5，1.5，3.0， 3.0 and 3.0 μg/mL，respectively. The detection limits were 0.5，0.5，0.5，1.0，1.0，1.0 μg/mL，respectively. RSDs of precision ， stability（12 h）and reproducibility tests were all lower than 2.0％. The average recoveries were 95.87％-98.59％（RSD＝1.04％，n＝ 9），95.66％-99.84％（RSD＝1.20％，n＝9），96.11％-98.97％（RSD＝1.04％，n＝9），95.06％-99.11％（RSD＝1.25％，n＝9）， 95.69％-98.22％（RSD＝0.83％，n＝9），95.34％-98.56％（RSD＝1.01％，n＝9）. The contents of 6 carbohydrate related substances in 9 batches of glucose were 1.26-2.22，2.55-3.36，2.37-3.37，1.28-2.01，0-2.11 and 0-1.89 mg/g，respectively. CONCLUSIONS ： Established method is accurate and sensitive ，and can be used for the detection of carbohydrate related substances in glucose.
ABSTRACT
OBJECTIVE：To establish a method for sim ultaneous determination of 7-hydroxycoumarin，6，7-dimethoxy- coumarin，5，7-dimethoxycoumarin，imperatorin and bergaptene in Shugan hewei pills. METHODS ：Samples were extracted by Soxhlet extraction and separated by using D 101 macroporous adsorption resin ；HPLC method was used to determine the contents of above 5 components. The determination was performed on Venusil MP C 18 column with mobile phase consisted of methanol- 0.1％ phosphoric acid water solution （gradient elution ）at the flow rate of 1.0 mL/min. The detection wavelength was 270 nm and the column temperature was 30 ℃ . The sample size was 10 μ L. RESULTS：The linear ranges were 1.875-187.5 μ g/mL for 7-hydroxycoumarin（r＝0.999 9），1.075-107.5 μg/mL for 6，7-dimethoxycoumarin（r＝0.999 9），1.261-126.1 μg/mL for 5， 7-dimethoxycoumarin（r＝0.999 9），0.875-87.5 μg/mL for imperatorin（r＝0.999 9），2.033-203.3 μg/mL for bergaptene（r＝0.999 8）， respectively. RSDs of precision ，stability（24 h），reproducibility and durability tests were lower than 2.0％. Average recoveries were 95.18％ -98.44％ （RSD＝1.27％ ，n＝6）， 95.35％ -98.14％ （RSD＝1.16％ ，n＝6），95.21％ -97.32％ （RSD＝0.83％ ，n＝6）， 95.43％-97.14％（RSD＝0.76％，n＝6），95.12％-98.75％（RSD＝1.35％，n＝6），respectively. The average contents of the above five components in 3 batches of shugan hewei pills were 0.424，0.239，0.305，0.180，0.459 mg/g（n＝2）.CONCLUSIONS：A method for simultaneous determination of five components in Shugan hewei pills was established.