Use of Ponkan mandarin peels as biosorbent for toxic metals uptake from aqueous solutions

Waste Ponkan mandarin (Citrus reticulata) peel was used as biosorbent to extract Ni(II), Co(II) and Cu(II) from aqueous solutions at room temperature. To achieve the best adsorption conditions the influence of pH and contact time were investigated. The isotherms of adsorption were fitted to the Langmuir equation. Based on the capacity of adsorption of the natural biosorbent to interact with the metallic ions, the following results were obtained 1.92, 1.37 and 1.31 mmol g(-1) for Ni(II), Co(II) and Cu(II), respectively, reflecting a maximum adsorption order of Ni(II)>Co(II)>Cu(II). The quick adsorption process reached the equilibrium before 5, 10 and 15 min for Ni(II), Co(II) and Cu(II), respectively, with maximum adsorptions at pH 4.8. In order to evaluate the Ponkan mandarin peel a biosorbent in dynamic system, a glass column was fulfilled with 1.00 g of this natural adsorbent, and it was fed with 5.00 x 10(-4)mol l(-1) of Ni(II) or Co(II) or Cu(II) at pH 4.8 and 3.5 ml min(-1). The lower breakpoints (BP(1)) were attained at concentrations of effluent of the column attained the maximum limit allowed of these elements in waters (>0.1 mg l(-1)) which were: 110, 100 and 130 bed volumes (V(effluent)/V(adsorbent)), for Ni(II), Co(II) and Cu(II), respectively. The higher breakpoints (BP(2)) were attained when the complete saturation of the natural adsorbent occurred, and the values obtained were: 740, 540 and 520 bed volumes for Ni(II), Co(II) and Cu(II), respectively.     

AB-8大孔吸附树脂精制芦柑皮总黄酮及黄酮类化合物的分离

目的：研究AB-8大孔吸附树脂精制芦柑皮总黄酮的工艺条件及芦柑皮黄酮类化合物的分离纯化。方法：采用AB-8大孔吸附树脂动态法精制芦柑皮总黄酮,考察上样液总黄酮质量浓度、pH值、上样流速、洗脱液乙醇体积分数对吸附解吸性能的影响;然后将精制的芦柑皮总黄酮经硅胶柱层析、半制备高效液相等技术进行分离纯化,并根据理化性质和波谱数据鉴定化学结构。结果：AB-8大孔树脂精制芦柑皮总黄酮的最佳工艺条件为上样液总黄酮质量浓度3.03 mg/mL、上样液pH 3.0、上样流速3.0 BV/h、洗脱液乙醇体积分数为90%,最优条件下可使芦柑皮总黄酮的纯度从17.8%提高到63.1%;此外,从精制的芦柑皮黄酮中分离到8 个黄酮类化合物,分别鉴定为：橘皮素、川陈皮素、4’,5,7,8-四甲氧基黄酮、5-去甲基-橘皮素、橙黄酮、橙浸膏、柚皮苷、橙皮苷。结论：AB-8大孔树脂能很好地富集纯化芦柑皮总黄酮,该法简单、可行;从精制的芦柑皮黄酮中分离到8 个黄酮类化合物,其中,4’,5,7,8-四甲氧基黄酮、5-去甲基-橘皮素、橙浸膏、柚皮苷、橙皮苷首次从芦柑皮中分得。     

纤维素酶提取湘西椪柑皮中总黄酮的工艺优化研究

采用响应面法对纤维素酶提取椪柑皮中总黄酮的工艺进行优化。结果表明,酶法提取椪柑皮总黄酮的最佳工艺条件为酶用量120U/mL、酶解温度52℃、酶解时间140min、酶解pH4.35,总黄酮得率可达1.85%。     

The methoxyflavones in Citrus reticulata Blanco cv. ponkan and their antiproliferative activity against cancer cells

The major polymethoxyflavones in the fruit (ponkan) peels of Citrus reticulata Blanco cv. ponkan were identified as isosinensetin, sinensetin, nobiletin and tetramethyl-o-scutellarein by a combined separation using high-speed countercurrent chromatography and preparative high performance liquid chromatography, and structure elucidation by electrospray ionisation mass spectrometry (ESI-MS) and ¹H and ¹³C nuclear magnetic resonance (NMR). The antiproliferative activity of the four compounds against four cancer cell lines (A549, HL-60, MCF-7 and HO8910) showed that isosinensetin had a lower IC₅₀ value for MCF-7 and HO8910 cancer cell lines. Determination of polymethoxyflavones in ponkan peels from different cultivation regions displayed relatively steady contents of the four compounds and a higher content of isosinensetin, which suggested that ponkan peels are excellent sources of functional polymethoxyflavones that may help prevent female cancers, such as ovarian cancer and breast cancer.     

响应面法优化椪柑果酒发酵工艺研究

以椪柑果汁为主要原料,酿酒高活性干酵母为发酵菌种,研究了椪柑果酒的发酵工艺。在单因素试验基础上,选取接种量、糖度、pH、发酵温度为影响因素,酒精度为响应值,应用中心组合 Box-Behnken 试验设计建立数学模型,进行响应面分析。研究结果表明,椪柑果酒发酵的最佳工艺为：接种量 0.11g/100ml、糖度 21%、pH3.6、发酵温度 26℃、发酵时间6d,在此工艺条件下,椪柑果酒酒精度达 9.5%（v/v）。     

椪柑果酒酿造工艺参数的优化

以啤酒酵母为试验菌株,以麻阳椪柑为原料,通过单因素试验和正交试验,研究了柑橘果酒的酿造工艺。结果表明,椪柑果酒酿造工艺条件为椪柑果汁初始糖度22%、啤酒酵母接种量7%、发酵温度22 ℃、椪柑果汁初始pH 4.0和发酵时间7 d;再经陈酿1个月并离心澄清（4 000 r/min,25 min）后,所得椪柑果酒酒精度为10.4%vol,残糖量为1.89%,椪柑果酒口味纯正、香气浓郁、澄清透明。     

紫胶涂膜常温贮藏对椪柑挥发性成分的影响

研究漂白紫胶涂膜处理对水果常温保鲜贮藏过程中香气成分的影响。用动态顶空密闭循环式吸附捕集法分别采集涂膜椪柑完整果实在贮藏期(涂膜后10～40d)的挥发物,并进行热脱附- 气相色谱/ 质谱(TCT-GC/MS)分析。结果表明,其完整果实挥发物中的香气组分均为萜烯类化合物及其衍生物,主要成分柠檬烯在对照样品挥发物中相对含量始终较低(可能挥发高峰在观测开始之前已出现过),均为(10 ± 3)%,而经6% 和12%漂白紫胶涂膜处理后在常温贮藏过程中挥发程度减缓(挥发高峰出现在观测阶段的早期),在挥发物中相对含量分别由10d 时的34.67% 和40.83%降至40d 时的14.64% 和11.69%,有利于保持柑橘类水果的特征香气状况;涂膜对挥发物的缓释作用可通过提高漂白紫胶浓度(即相应增加涂层厚度或致密度)加以强化;涂层厚度或致密度均匀性的改善可选择在较高浓度涂膜剂中添加纳米SiOx 材料,使缓释效果更加显著(挥发高峰出现在观测阶段的后期),柠檬烯在挥发物中相对含量从10～20d 期间均较低(分别为12.41% 和10.30%),至30d 时才增至19.29%,而至40d 时达到35.16%。     

共同定化多菌种发酵椪柑果醋工艺研究

以海藻酸钠为固定化材料,研究了多菌种（酿酒酵母、产香酵母、乳酸茵、醋酸菌）共固定化技术在椪柑果醋发酵中的应用。结果表明,固定化多菌种发酵椪柑果醋的最佳工艺条件为：酒精发酵阶段,接种量20％（v／v）、发酵温度32℃、时间60h、底物糖度23％;醋酸发酵阶段,接种量20％、发酵温度35℃、时间7d。所酿造的果醋具有椪柑的固有色泽、香气,无沉淀物,酸味柔和适中。     

椪柑果醋液态发酵工艺及香气成分的GC-MS分析

以椪柑为原料,通过正交试验设计研究酒精发酵和醋酸发酵的最优工艺。采用固相微萃取-气相色谱-质谱联用技术鉴定椪柑果醋中的挥发性风味物质,结果表明:椪柑果醋液态发酵最佳条件是:酿酒酵母添加量0.10%,发酵温度28℃,表观糖度18°Brix,醋酸接种量8%,发酵温度30℃,通气程度1/5。经GC-MS分析鉴定,液态发酵的椪柑果醋共含66种挥发性物质,其中乙酸是椪柑果醋中含量最高的挥发性成分,占风味总量的40.80%;酯类化合物是最主要的风味物质,占25.92%;柠烯是重要的特征香味组分,占2.74%。     

长波紫外造成货架椪柑汁挥发性风味组分的变化

研究了长波紫外线（ultraviolet-A,UVA）对非浓缩还原椪柑汁货架风味品质影响。PET瓶装椪柑汁于25 ℃货架上施以UVA照射30 d,同时以避光存放椪柑汁为对照。分别对0 d、避光30 d和UVA照射30 d椪柑汁,采用顶空固相微萃取-气相色谱-质谱/脉冲火焰光度检测联用法分析其挥发性物质的组成和含量差异,通过气味活性值（odor active value,OAV）筛选受UVA显著影响的风味组分,确定UVA照射对货架果汁整体风味的作用。结果显示,0 d、避光和UVA照射椪柑汁中分别检出43、51和53种挥发物。对避光和UVA照射终了样品中浓度存在显著差异的物质,筛选出OAV≥1的关键风味成分共22种,包括芳樟醇、苯乙醛、甲硫醚等6个醇、6个醛、4个烃、3个挥发性硫化物、2个酯及1个酮类物质;其中花香气味强度（以OAV计）0 d（583）>避光（456）>UVA（400）照射,不良风味强度反之（83、135和284）,并得到感官评价基本验证。此外,UVA还加速异味物质甲硫醚的生成。综上所述,UVA影响椪柑汁风味组分浓度变化,加速风味品质劣变。