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酒制延胡索微波炮制工艺的优化研究 Δ
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王 斌 1,2* ,梁伟龙 ,林钦贤 ,康志英 ,王其丰(1.广州市香雪制药股份有限公司,广州 510663;2.宁夏隆德
县六盘山中药资源开发有限公司,宁夏 固原 756300;3.亳州市沪谯药业有限公司,安徽 亳州 236800)
中图分类号 R283;R917 文献标志码 A 文章编号 1001-0408(2020)20-2503-05
DOI 10.6039/j.issn.1001-0408.2020.20.13
摘 要 目的:优化酒制延胡索的微波炮制工艺。方法:采用高效液相色谱法测定微波炮制酒制延胡索中原阿片碱、盐酸小檗碱、
延胡索乙素的含量;采用热浸法测定浸出物含量。在单因素试验的基础上,以微波炮制酒制延胡索的外观性状、浸出物和原阿片
碱、盐酸小檗碱、延胡索乙素含量为评价指标,以黄酒量、闷润时间、火力大小、炮制时间为考察因素,采用正交试验法结合综合加
权评分法优化炮制工艺并验证,同时与传统酒制延胡索进行比较。结果:原阿片碱、盐酸小檗碱、延胡索乙素检测进样量的线性范
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围分别为0.100~1.500 μg(R =0.999 6)、0.012~0.188 μg(R =0.999 5)、0.050~0.750 μg(R =0.999 8);精密度、稳定性(12 h)、重
复性试验的 RSD 均小于 2%;加样回收率分别为 99.15%~100.34%(RSD=0.54%,n=6)、99.52%~100.78%(RSD=0.69%,n=
6)、99.26%~99.79%(RSD=0.28%,n=6)。最优微波炮制工艺为黄酒用量4 g(约药材量的20%)、微波火力40%、闷润时间3 h、
炮制时间 3 min。3 次验证试验结果显示,浸出物、原阿片碱、盐酸小檗碱、延胡索乙素的含量分别为 15.7%~16.1%、0.061%~
0.063%、0.003%~0.004%、0.061%~0.063%;综合评分分别为97.916、94.730、97.217分,RSD分别为0.42%、0.38%、0.46%(n=3);
与传统酒制法比较,原阿片碱等成分的含量无显著性差异,但微波炮制酒制延胡索无焦斑、焦屑。结论:所建含量测定方法操作简便、
准确可靠、重复性好,可用于酒制延胡索中活性成分的定量分析;所得微波炮制工艺稳定、可行,可用于酒制延胡索的炮制。
关键词 微波炮制法;酒制延胡索;浸出物;原阿片碱;盐酸小檗碱;延胡索乙素;正交试验;高效液相色谱法
Optimization of the Microwave Processing Technology of Yellow Wine-processed Corydalis yanhusuo
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WANG Bin 1,2 ,LIANG Weilong ,LIN Qinxian ,KANG Zhiying ,WANG Qifeng (1. Guangzhou Xiangxue
Pharmaceutical Co.,Ltd.,Guangzhou 510663,China;2. Ningxia Longde County Liupanshan TCM Resource
Development Co.,Ltd.,Ningxia Guyuan 756300,China;3. Bozhou Huqiao Pharmaceutical Co.,Ltd.,Anhui
Bozhou 236800,China)
ABSTRACT OBJECTIVE:To optimize the microwave processing technology of yellow wine-processed Corydalis yanhusuo.
METHODS:The contents of opioid alkaloid,berberine hydrochloride and tetrahydropalmatine in C. yanhusuo processed with
yellow wine were determined by HPLC. The contents of the extracts were determined by hot dipping method. Based on the single
factor tests,using the appearance of yellow wine-processed C. yanhusuo with microwave processing technology,the contents of
extract,opioid alkaloid,berberine hydrochloride and tetrahydropalmatine as indexes,with the amount of yellow wine,wetting
time,microwave power and microwaving time as factors,the processing technology was optimized with orthogonal test combined
with comprehensive weighted scoring method,and then validated and compared with traditional yellow wine-processed C. yanhusuo.
RESULTS:The linear ranges of opioid alkaloid,berberine hydrochloride and tetrahydropalmatine were 0.100-1.500 μg(R =0.999 6),
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0.012-0.188 μg(R =0.999 5),0.050-0.750 μg(R =0.999 8). RSDs of precision,stability(12 h)and repeatability tests were all
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less than 2% . The recoveries were 99.15% -100.34%(RSD=0.54% ,n=6),99.52% -100.78%(RSD=0.69% ,n=6),
99.26%-99.79%(RSD=0.28%,n=6). The optimum microwave processing technology included that the amount of yellow wine
was 4 g(about 20% of medicinal material amount),microwave power was 40%,wetting time was 3 hour,processing time was 3
min. The results of three verification tests showed that the contents of extract,opioid alkaloid,berberine hydrochloride and
tetrahydropalmatine were 15.7%-16.1%,0.061%-0.063%,0.003%-0.004% and 0.061%-0.063%. The comprehensive scores were
97.916,94.730 and 97.217,and RSD were 0.42%,0.38%,0.46%(n=3),respectively. Compared with traditional yellow wine
processing technology,there was no significant difference in the contents of opioid alkaloid and other components,but no
scorched spot and crumbs was found in yellow wine-processed C. yanhusuo with microwave processing technology.
CONCLUSIONS:Established method for content determination is simple,accurate,reliable and reproducible,and can be used for
quantitative analysis of active components in yellow wine-processed C. yanhusuo. Optimized microwave processing technology is
stable and feasible,and can be used for the processing of
Δ 基金项目:国家中医药管理局中药重点产品行业标准制定计划
yellow wine-processed C. yanhusuo.
(No.国中医药法监函〔2017〕17号)
KEYWORDS Microwave processing technology; Yellow
*主管中药师,硕士。研究方向:中药饮片炮制及质量标准。电
话:020-22211159。E-mail:wangbin@xphcn.com wine-processed Corydalis yanhusuo;Extract;Opioid alkaloid;
# 通信作者:高级工程师。研究方向:中药新产品、新技术。电 Berberine hydrochloride; Tetrahydropalmatine; Orthogonal
话:020-22211304。E-mail:kangzhy@xphcn.com test;HPLC
中国药房 2020年第31卷第20期 China Pharmacy 2020 Vol. 31 No. 20 ·2503 ·