中国医药科学
中國醫藥科學
중국의약과학
CHINA MEDICINE AND PHARMACY
2014年
17期
18-22
,共5页
四味清口含片%质量标准%薄层色谱法%高效液相色谱法%桂皮醛%含量测定
四味清口含片%質量標準%薄層色譜法%高效液相色譜法%桂皮醛%含量測定
사미청구함편%질량표준%박층색보법%고효액상색보법%계피철%함량측정
Siweiqing buccal tablets%Quality standards%TLC%HPLC%Cinnamaldehyde%Content determination
目的：建立四味清口含片的质量控制标准。方法采用薄层色谱法(TLC)定性鉴别四味清口含片中的桂心、甘草、细辛、广陈皮，采用高效液相色谱法（HPLC）测定四味清口含片中桂皮醛的含量。色谱条件为Hypersil ODS（C18）色谱柱（4.6mm×250mm，5μm），检测波长为290 nm，流动相为甲醇-φ=0.1%磷酸水溶液(35∶65，v/v)，流速为1.0mL/min，柱温为30℃，理论板数以桂皮醛峰计算不低于3000。结果 TLC法能分别检出四味清口含片中桂心（肉桂）、甘草、细辛、广陈皮，均具有良好的鉴别特征，阴性未见干扰；桂皮醛进样量在0.010～0.500μg 范围内与峰面积积分值线性关系良好，r=0.9999。在精密度试验、稳定性试验、重复性试验中峰面积的相对标准偏差（RSD）分别为1.03%、1.27%、1.23%。加样回收率为97.23%～101.54%，平均值为99.43%，RSD为0.99%（n=9）。结论本方法具有良好的专属性和重现性，加样回收率试验符合要求，能准确、稳定地对四味清口含片进行定性鉴别和定量测定，可用于该制剂的质量控制。
目的：建立四味清口含片的質量控製標準。方法採用薄層色譜法(TLC)定性鑒彆四味清口含片中的桂心、甘草、細辛、廣陳皮，採用高效液相色譜法（HPLC）測定四味清口含片中桂皮醛的含量。色譜條件為Hypersil ODS（C18）色譜柱（4.6mm×250mm，5μm），檢測波長為290 nm，流動相為甲醇-φ=0.1%燐痠水溶液(35∶65，v/v)，流速為1.0mL/min，柱溫為30℃，理論闆數以桂皮醛峰計算不低于3000。結果 TLC法能分彆檢齣四味清口含片中桂心（肉桂）、甘草、細辛、廣陳皮，均具有良好的鑒彆特徵，陰性未見榦擾；桂皮醛進樣量在0.010～0.500μg 範圍內與峰麵積積分值線性關繫良好，r=0.9999。在精密度試驗、穩定性試驗、重複性試驗中峰麵積的相對標準偏差（RSD）分彆為1.03%、1.27%、1.23%。加樣迴收率為97.23%～101.54%，平均值為99.43%，RSD為0.99%（n=9）。結論本方法具有良好的專屬性和重現性，加樣迴收率試驗符閤要求，能準確、穩定地對四味清口含片進行定性鑒彆和定量測定，可用于該製劑的質量控製。
목적：건립사미청구함편적질량공제표준。방법채용박층색보법(TLC)정성감별사미청구함편중적계심、감초、세신、엄진피，채용고효액상색보법（HPLC）측정사미청구함편중계피철적함량。색보조건위Hypersil ODS（C18）색보주（4.6mm×250mm，5μm），검측파장위290 nm，류동상위갑순-φ=0.1%린산수용액(35∶65，v/v)，류속위1.0mL/min，주온위30℃，이론판수이계피철봉계산불저우3000。결과 TLC법능분별검출사미청구함편중계심（육계）、감초、세신、엄진피，균구유량호적감별특정，음성미견간우；계피철진양량재0.010～0.500μg 범위내여봉면적적분치선성관계량호，r=0.9999。재정밀도시험、은정성시험、중복성시험중봉면적적상대표준편차（RSD）분별위1.03%、1.27%、1.23%。가양회수솔위97.23%～101.54%，평균치위99.43%，RSD위0.99%（n=9）。결론본방법구유량호적전속성화중현성，가양회수솔시험부합요구，능준학、은정지대사미청구함편진행정성감별화정량측정，가용우해제제적질량공제。
Objective To establish the quality control standard of Siweiqing buccal tablets. Methods Thin layer chromatography (TLC) was used to identify Cortex Cinnamomi, radix glycyrrhizae, Citrus Chachiensis Hortorum and Asarum heterotropoides Fr. Schmidt var. mandshuricum (Maxim.) Kitag. in these tablets preparation. The high performance liquid chromatography (HPLC) was adopted to determine the content of cinnamaldehyde. The chromatographic conditions were as follows: the chromatographic column Hypersil ODS(C18)column (4.6mm×250mm, 5μm), the detection wavelength of 290nm, the mobile phase of methanol-φ=0.1% phosphoric acid (35∶ 65, v/v), the flow velocity of 1.0mL/min, the column temperature at 30℃, the theoretical plate number no less than 3000. Results Citrus Chachiensis Hortorum, radix glycyrrhizae, Cortex Cinnamomi and Asarum heterotropoides Fr. Schmidt var. mandshuricum (Maxim.) Kitag. can be identified by TLC without interference of negative samples. The linear relationship between content of cinnamaldehyde and peak area was obtained during the range of 0.010-0.500μg, r=0.999 9. RSD's found of the peak area for the precision test, the stability test and the repeatability test were 1.03%, 1.27% and 1.23%, respectively. The recoveries of cinnamaldehyde obtained were in the range of 97.23%-101.54% and the average of 99.43% withRSDof 0.99% (n=9).Conclusion The method can be applied to qualitative identification and quantitative assay of Siweiqing buccal tablets with good reproducibility. The sampling recovery test is in compliance with the requirement. The quality standard can effectively control the quality of Siweiqing buccal Tablets with good specificity, reproducibility and stability. It can be applied to the quality control of Siweiqing buccal tablets.
