大黄趁鲜加工工艺:定尺寸饮片的研制及其质量评价

Development and evaluation for a new manufacturing technique of fixed size raw rhubarb decoction pieces

目的探索大黄原药材趁鲜加工成为定尺寸饮片的可行性及其质量评价。方法清洗鲜大黄药材,主根分离,去皮,先纵切成厚度为5 mm的薄片,再将薄片切制为长×宽=8 mm×8 mm的定尺寸饮片,将切制好的饮片平铺置于自动恒温鼓风式干燥箱内,干燥温度设定为45℃,连续干燥8 h,自然冷却,检定,即得生大黄定尺寸饮片。采用UPLC法测定大黄定尺寸饮片放置1年前后总游离蒽醌和番泻苷A、B的量,评价其质量稳定性。测定饮片中黄曲霉毒素、农药残留量、重金属残留量等指标评价其质量安全性。通过测定调剂称量误差范围来评价其调剂精准性。通过测定在水沸腾后煎煮10 min内番泻苷A的煎煮溶出曲线(煎煮溶出率)来评价其煎煮顺应性。考察了大黄定尺寸饮片炮制成为酒大黄、熟大黄和大黄炭的工艺可行性。结果结果显示,大黄药材具备趁鲜加工成为定尺寸饮片的工艺可行性。趁鲜加工后游离蒽醌总量和番泻苷A、B的保留率分别为96.92%、93.27%、91.67%,大黄定尺寸饮片室温放置1年后,游离蒽醌总量和番泻苷A、B的保留率分别为90.47%、86.59%、81.82%,表明其有效成分的保留率较高。趁鲜加工而成的定尺寸饮片中均未检测出农药残留,也未见重金属超标。连续称量6次大黄定尺寸饮片的RSD值为0.62%,而连续称量6次大黄常规饮片的RSD值为8.56%。箱形图显示,大黄定尺寸饮片的6次称量值的分布范围均匀,离异值极小。与大黄常规饮片相比,大黄定尺寸饮片中番泻苷A具有快速溶出、溶出率较高的特点。大黄定尺寸饮片可以炮制成为酒大黄、熟大黄和大黄炭。结论大黄药材趁鲜加工成为生大黄定尺寸饮片具备可行性,可避免由于干燥不及时导致的发霉变质现象,可降低有效成分的流失,缩短了生产周期,并提高了调剂精准性,质量稳定性良好。以鲜大黄药材趁鲜加工制备而成的定尺寸饮片具有品质道地性、质量稳定性、规格均一性、调剂精准性等特点,并具备加工成为不同炮制品的可行性。

Objective To explore the feasibility of rhubarb being processed into fixed size decoction pieces. Methods Firstly, fresh raw rhubarb was cleaned, and the skin was scraped off. Secondly, it was longitudinally cut up into 5 mm slices, then length × width = 8 mm × 8 mm fixed size decoction pieces. Thirdly, it was put into the automatic constant temperature blower box, and the drying temperature was set at 45 ℃ for 8 h; The fixed size decoction pieces were obtained after quality verification. In order to evaluate its quality stability, ultra-high performance liquid chromatography（UPLC） method was used to determine total free anthraquinone derivatives, sennoside A, and sennoside B in rhubarb before and after 1 year. Its quality security, quantitative determination of aflatoxin, pesticide residues, and heavy metal residues in rhubarb were evaluated. Weighing error range was used to evaluate the weighing precision of different rhubarb decoction pieces. Decoction dissolution curve of sennoside A within 10 minutes was used to evaluate its decoction compliance property and explore the feasibility of processing into different processed products. Results The results showed that it was feasible for raw rhubarb to become the fixed size decoction pieces. After the fresh processing, the conservation ratios of total free anthraquinones, sennoside A, and sennoside B were 96.92%, 93.27%, and 91.67%, respectively. The conservation ratios of total free anthraquinones, sennoside A, and sennoside B were 90.47%, 86.59%, and 81.82% after 1 year in the room temperature environment, which indicated that the conservation ratio of these bioactive ingredients were higher. No pesticide residues were detected in the fixed size decoction pieces of raw rhubarb, and no heavy metals were found to exceed the prescribed limits. The RSD value of continuous weighing six times for the fixed size raw rhubarb decoction pieces was 0.62%, while the RSD value of conventional raw rhubarb decoction pieces was 8.56%. The box-plot showed that the weighing error of the fixed size raw rhubarb decoction pieces was minimal. Compared with conventional rhubarb decoction pieces, sennoside A in the fixed size raw rhubarb decoction pieces has the characteristics of rapid dissolution and high dissolution rate. The fixed size raw rhubarb decoctionpieces could be processed into wine-treated rhubarb, ripe rhubarb, and rhubarb charcoal. Conclusion All results show that it has processing feasibility of fresh raw rhubarb, and it can avoid mildew phenomenon, can reduce the loss of active ingredients, shorten the production cycle, enhance the accuracy of the weighing, and is conducive to the quality maintain stable. These fixed size rhubarb decoction pieces have advantage of good quality genuine characteristic, superior quality stability, predominant size uniformity, and it has the good weighing accuracy and feasibility of processing to different rhubarb processed products.