ABSTRACT
OBJECTIVE：To establish a method for the simultan eous determination of the contents of 12 flavonoids in Quzhiqiao. METHODS ：HPLC method was adopted. The determination was performed on Agilent Extend C 18 column with mobile phase consisted of 0.1％ formic acid-acetonitrile （gradient elution ）at the flow rate of 1.0 mL/min. The column temperature was set at 35 ℃. The detection wavelength was set at 330 nm，and sample size was 10 μL. The contents of 12 components（such as eriocitrin，narirutin，naringin，naringenin，hesperidin，neohesperidin，hesperide hydrate ，luteolin，hesperide，nobiletin，hesperetin and hesperidolactone ）in 10 batches of Quzhiqiao from different collection places were determined. RESULTS ：The linear range of eriocitrin，narirutin，naringin，naringenin，hesperidin，neohesperidin，hesperide hydrate ，luteolin，hesperide，nobiletin，hesperetin and hesperidolactone were 1.65-16.51，4.50-45.02，35.41-354.12，4.11-41.12，2.29-22.86，34.96-349.56，1.42-14.15，1.50-15.04， 1.83-18.28，1.51-15.08，1.61-16.12，1.28-12.84 μg/mL，respectively（all r＞0.999 7）. The detection limits were 0.165 1，0.450 2， 3.541 2，0.411 2，0.228 6，3.495 6，0.141 5，0.150 4，0.182 8，0.150 8，0.161 2，0.128 4 μg/mL，respectively. The limits of quantitation were 0.547 8，1.487 4，11.663 3，1.360 3，0.758 3，11.594 9，0.466 3，0.497 1，0.601 2，0.499 9，0.532 3，0.424 6 μg/mL，respectively. RSDs of precision （n＝6），reproducibility（n＝6）and stability （24 h，n＝7）tests were all lower than 3％. The average recoveries were 99.50％，99.61％，98.18％，98.85％，98.48％，98.50％，98.25％，99.91％，103.13％，98.82％， 98.44％ ， 100.29％ （RSD＝1.49％ -2.38％ ， n＝6）. The contents of the above 12 components in 10 batches of samples from different collection places were 1.995 5-2.648 8，4.317 7- 5.005 1，33.215 5-34.054 6，3.140 4-3.471 5，3.221 2-3.748 8， 42.746 6-44.026 6，0.202 7-0.239 4，0.191 2-0.208 8，0.080 3- 0.097 9，0.291 9-0.307 1，0.119 9-0.149 1，0.082 7-0.089 8 mg/g. CONC LUSIONS：The method is accurate ，reliable，simple and efficient，which can be used to simultaneous determination of the contents of 12 flavonoids in Quzhiqiao ，and to provide reference for the establishment of quality control standards of Quzhiqiao.
ABSTRACT
OBJECTIVE: To determine the mass scores of naringin and neohesperidin in Fructus aurantii and Citrus chang-shan-huyou with their processed products and evaluate the quality of Fructus aurantii and Citrus changshan-huyou with their pro-cessed products. METHODS:According to the requirements of Chinese Pharmacopoeia(2010 edition)and Zhejiang Province Tradi-tional Chinese Medicine Preparation Standards (2005 edition),the moisture and ash of F. aurantii and C. changshan-huyou with their processed products were detected. And the contents of naringin and neohesperidin were determined. The ZORBAX SB-C18 column was used with the mobile phase of acetonitrile-water(20∶80,V/V)at the flow rate of 1.0 ml/min. The detection wave-length was set at 283 nm,and the column temperature was 40℃.The samples size was 10μl. RESULTS:The moisture of F. au-rantii and C. changshan-huyou was decreased after processing with no obvious change for ash. The contents of naringin and neohes-peridin were decreased,significantly for F. aurantii,and all consistent with the requirements of Chinese Pharmacopoeia(2010 edi-tion)except F. aurantii. The linear range was 0.028 45-0.284 5μg(r=0.999 7)for naringin and 0.085 9-0.858 6μg(r=0.999 6)for neohesperidin;the RSDs of precision,stability and reproducibility tests were no more than 1.36% and the average recovery was re-spectively 96.45%-100.43%(RSD=1.45%,n=6) and 98.36%-102.00%(RSD=1.26%,n=6). CONCLUSIONS: There was no significant difference in the inspection and determination re-sults in F. aurantii and C. changshan-huyou. It is suggested to adjust the limitation of content determination in the Chinese Pharmacopoeia(2010 edition)and processed standards.
ABSTRACT
OBJECTIVE:To establish the HS-GC method for the content determination of menthol in Qiangli Pipa syrup,and the content of menthol in 56 batches of Qiangli Pipa syrup commercially available was determined. METHODS:HS-GC was per-formed on the column of Agilent HP-INNOWAX,column temperature was 130 ℃(maintaining 7 min),FID was used as detector, inlet temperature was 200 ℃,detector temperature was 250 ℃,carrier gas was high-purity nitrogen,flow rate was 3 ml/min,split ratio was 10∶1 and the injection volume was 1 000 μl. RESULTS:The linear range of menthol was 0.007 07-0.141 40 mg/ml(r=0.999 1);RSDs of precision,reproducibility and stability tests were no more than 3.37%;average recovery was 94.3%-99.6%(RSD=1.86%,n=6). There was significant difference in the contents of menthol in 56 batches Qiangli Pipa syrup. CONCLU-SIONS:The method is simple,sensitive,accurate and reliable,and can be used for content determination of menthol in Qiangli Pi-pa syrup. The sampling results show it is necessary to update the detecting items for the content of Qiangli pipa loquat and strength-en the quality control of it.