RESUMO
OBJECTIVE To establish a quality standard for rice-fired Glehnia littoralis . METHODS Appearance observation , powder microscopic identification and thin-layer chromatography (TLC)identification were performed for the samples of rice-fired G. littoralis decoction piece. According to the relevant methods stated in 2020 edition of Chinese Pharmacopoeia (part Ⅳ),the contents of moisture ,total ash ,acid-insoluble ash ,water-soluble extract and acid-soluble extract were determined. The contents of psoralen,zanthoxylin,bergapten,imperatorin and isoimperatorin were determined by high performance liquid chromatography (HPLC). RESULTS The rice-fired G. littoralis decoction pieces were round-like small segments ,slightly rough ,yellow(peeled) or dark yellowish brown (with peel ),special gas and slightly sweet taste. The powder was yellowish white. Under the microscope , secretions and secretory cells ,ducts,gelatinized starch granules ,ray cells ,parenchyma cells ,etc. could be seen. TLC showed the spots developed clearly. In the chromatogram of the test sample ,there was the same blue fluorescent spot at the corresponding position of the chromatogram of isoimperatorin control sample. The moisture ,total ash ,acid-insoluble ash ,water-soluble extract and ethanol-soluble extract from 9 batches of samples were 5.82%-6.27%,3.19%-3.59%,0.21%-0.27%,24.91%-30.30% and 20.66% -25.83% ,respectively. The linear range of psoralen ,zanthotoxin,bergapten,imperatorin and isoimperatorin were 0.240-2.400,0.320-3.200,0.224-2.240,0.292-2.920,0.208-2.080 µg/mL(all r>0.999 0). Limits of quantitation were 0.032 0, 0.030 0,0325 0,0.032 0,0.045 0 µg,respectively. Limits of detection were 0.100 8,0.089 6,0.071 5,0.090 0,0.132 0 µg, respectively. RSDs of prescision ,stability(24 h)and reprodu- cibility tests were less than 3%. Average recoveries were 100.56% (RSD=1.36% ,n=6),100.73%(RSD=2.25% ,n=6), 100.36%(RSD=0.98%,n=6),98.24%(RSD=0.40%,n=6) E-mail:853063968@qq.com and 99.40%(RSD=0.35%,n=6),respectively. The contents of above five components were 5.85-13.31,8.63-33.38,6.23- E-mail:shixiaofeng2005@sina.com 15.25,6.12-12.98,5.52-10.77 µg/g,respectively. The total contents were 34.20-83.47 µg/g. CONCLUSIONS It is preliminarily proposed that the moisture ,total ash and acid-insoluble ash should not exceed 7.30%,4.10%,0.30%. The water-soluble extract and ethanol-soluble extract are no less than 21.00% and 18.00%,respectively. The total content of coumarin should not be less than 52.03 µg/g(with peel )and 26.34 μg/g(peeled). Established quality standard can be used for the quality control of rice-fired G. littoralis .