基于CRITIC法优化大叶冬青瞬时高温灭菌工艺

doi:10.13304/j.nykjdb.2023.0055

摘要/Abstract

摘要：

为优化大叶冬青瞬时高温灭菌工艺，分析其对大叶冬青灭菌效果及质量的影响，采用正交试验法，研究灭菌前后大叶冬青1，1-二苯基-2-苦基肼（1，1-Diphenyl-2-picrylhydrazyl， DPPH）自由基清除率及多酚类化合物和皂苷类化合物含量的变化，以灭菌温度、灭菌时间、药材粒度为考察因素，以灭菌率、DPPH自由基清除率、多酚类、皂苷类化合物含量为评价指标，通过权重分析法（criteria importance though intercrieria correlation，CRITIC）确定指标相关性权重并计算综合评分。结果表明，按照综合加权法确定的权重系数是多酚类化合物含量25.78%、皂苷类类化合物含量47.22%、DPPH·清除率26.99%，最佳灭菌工艺条件为：灭菌温度160或170 ℃，灭菌时间10 s，粉碎粒度不大于24目。按优化工艺灭菌后的样品微生物限度检查均符合药典规定；灭菌前后样品的多酚、皂苷类化合物含量及DPPH自由基清除率均无明显变化，且样品多酚、皂苷类化合物的指纹图谱相似度≥0.9。综上所述，瞬时高温灭菌能有效杀灭大叶冬青中的微生物，且对质量无影响。

关键词: 大叶冬青, 瞬时高温灭菌, 正交设计, 抗氧化活性, 多酚类化合物, 皂苷类化合物

Abstract:

To optimize the instantaneous high temperature sterilization process of Ilexmacrophylla and investigate its effect on the sterilization effect and quality of Ilex latifolia， the orthogonal experiment was used. The changes of 1，1-dipheny l-2-picrylhydrazyl （DPPH） free radical clearance rate and the contents of polyphenolic compounds and saponins in Ilex latifolia before and after sterilization. The instantaneous high temperature sterilization process of Ilexmacrophylla was optimized， with the sterilization temperature， sterilization time and medicinal material particle size as the investigation factors， and the sterilization rate， DPPH·clearance rate， contents of polyphenols and saponins as the evaluation indicators. The correlation weight of indicators was determined by criteria importance though intercrieria correlation （CRITIC） method to calculate the comprehensive score. The results showed that， according to the comprehensive weighting method， the weight coefficient of polyphenols， saponins and of DPPH·clearance rate were 25.78%， 47.22% and 26.99%， respectively. The optimal sterilization process was as follows： sterilization temperature 160～170 ℃， sterilization time 10 s， and grinding size no more than 24 mesh. The microbial limits of the samples after sterilization with the optimized process were in accordance with the provisions of pharmacopoeia. And compared with before sterilization， there were no significant changes in the contents of polyphenols， saponins and DPPH·clearance rate after sterilization， the fingerprints of polyphenols and saponins after sterilization of samples were similar with before sterilization， with similarity ≥0.9. In conclusion， instantaneous high temperature sterilization could effectively kill the microorganisms in Ilex latifolia， and had no effect on the quality.

Key words: Ilex latifolia Thunb., instant high temperature sterilization, orthogonal design, antioxidant activity, polyphenols, saponins

中图分类号:

S567.1

刘融融, 焦连庆, 张婷, 于敏, 田义新. 基于CRITIC法优化大叶冬青瞬时高温灭菌工艺[J]. 中国农业科技导报, 2023, 25(12): 205-215.

Rongrong LIU, Lianqing JIAO, Ting ZHANG, Min YU, Yixin TIAN. Optimization of Instantaneous High-temperature Sterilization Process Before and After Sterilization of Ilex latifolia Based on CRITIC Method[J]. Journal of Agricultural Science and Technology, 2023, 25(12): 205-215.

图/表 12

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样品序号 Sample number	A：温度 Temperature/℃	B：时间 Time/s	C：粒度/目 Fineness/mesh	D：空白 Blank	灭菌率 Sterilization rate/%
1	140	5	80		88.62
2	140	10	24		92.43
3	140	15	50		90.29
4	160	5	24		95.88
5	160	10	50		96.10
6	160	15	80		96.83
7	180	5	50		96.64
8	180	10	80		98.01
9	180	15	24		97.97
K1	90.447	93.713	94.487	94.230
K2	96.270	95.513	95.472	95.300
K3	97.540	95.030	96.343	94.727
R	7.093	1.800	1.084	1.070

样品序号 Sample number	A：温度 Temperature/℃	B：时间 Time/s	C：粒度/目 Fineness/mesh	D：空白 Blank	灭菌率 Sterilization rate/%
1	140	5	80		88.62
2	140	10	24		92.43
3	140	15	50		90.29
4	160	5	24		95.88
5	160	10	50		96.10
6	160	15	80		96.83
7	180	5	50		96.64
8	180	10	80		98.01
9	180	15	24		97.97
K1	90.447	93.713	94.487	94.230
K2	96.270	95.513	95.472	95.300
K3	97.540	95.030	96.343	94.727
R	7.093	1.800	1.084	1.070

方差来源 Soruce of variation	离差平方和 Sum of square	自由度 df	方差 Variance	F值 F value
A：温度Temperature	85.839	2	42.920	49.898^*
B：时间 Time	5.207	2	2.604	3.027
C：粒度Fineness	2.078	2	1.039	1.208
误差Error	8.040	2	4.020

方差来源 Soruce of variation	离差平方和 Sum of square	自由度 df	方差 Variance	F值 F value
A：温度Temperature	85.839	2	42.920	49.898^*
B：时间 Time	5.207	2	2.604	3.027
C：粒度Fineness	2.078	2	1.039	1.208
误差Error	8.040	2	4.020

多酚类 Polyphenol	样品Sample
多酚类 Polyphenol	1号 No. 1	2号 No.2	3号 No.3	4号 No.4	5号 No.5	6号 No.6	7号 No.7	8号 No.8	9号 No.9
新绿原酸 Neochlorogenic acid	0.081 6	0.067 1	0.070 9	0.079 9	0.073 0	0.073 4	0.071 2	0.075 1	0.077 9
绿原酸 Chlorogenic acid	0.263 6	0.223 2	0.246 6	0.268 0	0.238 8	0.247 1	0.239 5	0.245 1	0.255 0
隐绿原酸 Cryptochlorogenic acid	0.100 9	0.087 5	0.091 0	0.106 3	0.096 4	0.096 4	0.093 1	0.098 1	0.099 2
咖啡酸 Caffeic acid	0.00 18	0.001 8	0.000 7	0.000 7	0.003 7	0.001 3	0.000 8	0.001 0	0.000 8
对羟基肉桂酸 P-hydroxycinnamic acid	0.002 4	0.002 5	0.001 6	0.002 1	0.004 7	0.001 8	0.001 7	0.002 7	0.001 4
芦丁 Rutin	0.104 0	0.138 4	0.122 3	0.158 3	0.141 5	0.128 2	0.126 9	0.125 3	0.126 0
异槲皮素 Isoquercetin	0.010 1	0.014 1	0.011 0	0.014 5	0.015 7	0.012 4	0.012 0	0.012 7	0.012 3
异绿原酸B Isochlorogenic acid B	0.009 4	0.005 3	0.008 7	0.005 6	0.009 3	0.008 4	0.008 7	0.010 8	0.009 8
异绿原酸A Isochlorogenic acid A	0.082 4	0.066 9	0.085 9	0.074 0	0.073 3	0.082 0	0.076 8	0.075 5	0.076 5
异绿原酸C Isochlorogenic acid C	0.045 7	0.056 7	0.072 2	0.065 4	0.066 5	0.072 7	0.064 6	0.068 0	0.071 7
总量 Total content	0.701 8	0.663 5	0.711 0	0.774 9	0.722 9	0.723 7	0.695 3	0.714 4	0.730 6