固相萃取-高效液相色谱法测定蔬菜水果中的氨基甲酸酯杀虫剂及其代谢物残留

采用乙腈提取-固相萃取浓缩 高效液相色谱分离 柱后衍生-荧光检测法测定了蔬菜 水果中8种氨基甲酸酯类杀虫剂及其代谢物残留量。采用加标法(添加水平为0.10,0.50mg/kg)测定了氨基甲酸酯杀虫剂及其代谢物的回收率,其平均回收率为70%-120%,相对标准偏差(RSD)小于20%(n=3),最低检出限范围为0.0042-0.0106 mg/kg。该方法的测定结果满足多残留农残的检测要求。     

改性柑橘果胶的制备、表征及抗癌活性

采用琼脂糖凝胶电泳、比旋度测试、HPSEC-RID、IR、¹H NMR、¹³C NMR、高碘酸氧化及甲基化分析等手段对改性柑橘果胶(MCP)进行了分析, 结果表明, MCP是一种均一性多糖, 分子量约为21000~66000, 糖醛酸质量分数为81.0%, 酯化度为2.13%. MCP的中性单糖残基主要包括鼠李糖(Rha)、阿拉伯糖(Ara)、木糖(Xyl)和半乳糖(Gal)等, 其摩尔比约为1.0∶1.5∶1.4∶1.3, 主链包括HG和RG, 分支结构含有末端Gal, Xyl和Ara. 选用3种小鼠移植性肿瘤模型对MCP的抗肿瘤生长活性进行研究. 结果表明, MCP对肝癌H22细胞有较强抑制作用, 高剂量下抑制率可达47.8%; 对宫颈癌U14细胞的抑制率在高剂量及中等剂量下分别达到36.5%和38.5%; 对肉瘤S180没有抑制活性. MCP的抗肝癌和抗宫颈癌活性为首次发现.     

优良发酵果蔬原酱专用乳酸菌的筛选及鉴定

采用目的平板梯度稀释法,从自然发酵果蔬原浆及中外泡菜老液中分离到22株乳酸菌。采用MRS(pH2.0)初筛平板和MRS(30%葡萄糖)复筛平板,筛选出4株耐酸、耐高糖乳杆菌。对其进行了pH值、酸度、活菌数等果蔬酱发酵性能测试研究,其中两株发酵产酸速度快、发酵性能优异、发酵果蔬酱风     

Elemental Analysis of Stone Fruits by Inductively Coupled Plasma Mass Spectrometry and Direct Mercury Analysis

This study reports the concentrations of eight trace essential (Zn, Mn, Cu, Ni, Cr, Co, V, and Se) and four toxic elements (Pb, As, Cd, and Hg) in commonly consumed stone fruits from South Korea. The samples were digested by microwave-induced combustion and analyzed by inductively coupled plasma mass spectrometry (ICP-MS). The concentrations of mercury were analyzed by direct mercury analysis (DMA). The analytical techniques were validated by linearity, limits of detection and quantification, precision, recovery, and for accuracy by analyzing a spinach leave-certified reference material; satisfactory results were obtained in all cases. The concentrations of essential trace elements varied considerably among the stone fruits. Generally stone fruits contained comparatively high concentrations of Zn (0.946 to 7.86?µg/g) and Mn (below the limit of detection to 1.66?µg/g), while lower contents of Cu (0.214 to 1.24?µg/g), Cr (0.032 to 0.114?µg/g), Ni (0.006 to 0.091?µg/g), Co (0.004 to 0.016?µg/g), V (below the limit of detection to 0.023?µg/g), and Se (0.0002 to 0.005?µg/g) were obtained. The concentrations (µg/g) of toxic metals were 0.007 (peach) to 0.016 (cherry) for Pb, 0.001 (plum) to 0.007 (cherry) for As, 0.002 (apricot and cherry) to 0.003 (peach) for Cd, and 0.0003 (peach) to 0.0016 (jujube) for Hg. The values for the estimated dietary intakes, target hazard quotients, and hazard indices were lower than the recommended safety limits by World Health Organization. Therefore, the analyzed stone fruits were deemed to be safe for human consumption.     

柱前衍生/高效液相色谱法测定果蔬中仲丁胺残留

建立了高效液相色谱(HPLC)测定仲丁胺的分析方法。试样采用全自动凯氏定氮仪蒸馏,蒸馏液经碱中和,以9-氯甲酸芴甲酯(FMOC)为衍生剂在碱性条件下衍生,衍生产物经C18柱分离,紫外检测器(265nm)检测。实验考察了衍生剂浓度、硼酸盐缓冲溶液的p H值、反应温度与时间等因素对衍生反应的影响,结果表明,最优的衍生剂浓度为0.50 g/L,缓冲溶液p H值为8.0,反应温度为室温,反应时间为15 min。在此条件下,仲丁胺在0.001~1.000 mg/L浓度范围内与其响应信号呈良好的线性关系,相关系数为0.999 8,加标回收率为82.4%~95.2%,相对标准偏差为1.3%~6.8%,方法检出限为0.1μg/kg,定量下限为0.5μg/kg。该方法快速、简便、安全、灵敏度高、重现性好,可用于果蔬中仲丁胺残留的测定。     

气相色谱-质谱法测定蔬菜与水果中11种三唑类农药残留

建立了蔬菜和水果中11种三唑类农药残留的气相色谱-质谱(GC - MS)测定方法.样品用乙腈均质提取,经石墨化炭黑/氨基复合柱净化,乙腈-甲苯(3:1)洗脱.洗脱液经浓缩、溶剂交换后定容,采用气相色谱-质谱的选择离子监测方式( GC - MSD/SIM)进行测定,内标法定量.方法的线性范围为0.05～5 ng,相关系数...     

Quantification of Flavonoids,Phenols and Antioxidant Potential from Dropped Citrus reticulata Blanco Fruits Influenced by Drying Techniques

Physiologically dropped immature Citrus reticulata Blanco fruits are regarded as waste and discarded in the citrus orchard but are a good source of bioactive compounds including flavonoids, antioxidants and total phenols. A study was undertaken to identify and quantify these bioactive compounds and to investigate the influence of different drying techniques, namely freeze drying and hot air oven drying, on flavonoids namely flavanone glycosides, antioxidant potential and total phenol content in immature dropped fruits of Citrus reticulata Blanco. Flavonoids were quantified in high-performance liquid chromatography (HPLC). The antioxidant activity were investigated with three assays azino-bis [3-ethylbenzthiazoline-6-sulfonic acid]) (ABTS), 2,2-diphenyl-1-picrylhydrazyl radical (DPPH), Ferric Reducing Ability of Plasma (FRAP) and total phenol content was determined. Freeze dried samples of 12 and 14 mm size retained maximum hesperidin flavonoid content (27.03% and 27.20%) as compared to the hot air dried samples (17.99%) and retained higher phenolic content ranged from 50.54–54.19 mg GAEL⁻¹. The antioxidant activity in freeze dried fruits was from 12.21–13.55 mM L⁻¹ Trolox and 15.27–16.72 mM L⁻¹ Trolox with ABTS, DPPH assay and FRAP values ranging from 7.31–9.07 mM L⁻¹ Trolox. Significant positive correlation was found between the flavonoid hesperidin with antioxidant assays and total phenolic content (TPC). The results showed that waste citrus fruits can act as potential source of bioflavonoids, especially hesperidin, and antioxidants for pharmaceutical as well as nutraceutical industry.     

Efficient analysis of phytochemical constituents in the peel of Chinese wild citrus Mangshanju (Citrus reticulata Blanco) by ultra high performance liquid chromatography–quadrupole time‐of‐flight‐mass spectrometry

An efficient ultra high‐performance liquid chromatography coupled with quadrupole time‐of‐flight mass spectrometry method was developed for separation and profiling of phytochemical constituents of Chinese wild mandarin Mangshanju (Citrus reticulata Blanco). All constituents were well separated within 16 min. Based on retention times, accurate mass, MS^E fragments, and/or reference standards as well as databases, a total of 81 compounds were unambiguously identified or tentatively assigned including flavonoid glycosides, acylated flavonoid glycosides, flavones, polymethoxylated flavonoids, and limonoids as well as four other compounds. Among them, 22 polymethoxylated flavones and ten polymethoxylated flavanones/chalcones were identified in Mangshanju, more types than other citrus reported before. A basic procedure for identifying flavonoid‐O‐glycosides and the aglycones including polymethoxylated flavonoids was proposed. In addition, this method was successfully used to analyze another four mandarin germplasms, Cenxi suan ju, Xipi gousi gan, Nanfeng miju, and Or, showing that Mangshanju contained two characteristic compounds distinct from the other four citrus species. This study systematically profiled phytochemical constituents of Mangshanju, which was helpful for further utilization of Mangshanju owing to its abundant bioactive compounds.     

固相萃取/超高效液相色谱-串联质谱测定水果中5种植物生长调节剂残留量

建立了固相萃取/超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定水果中6-苄基腺嘌呤(6-BA)、噻苯隆、氯吡脲、多效唑和烯效唑5种植物生长调节剂残留量的分析方法。水果样品经乙腈提取,NH2固相萃取小柱进行富集、净化,以二氯甲烷-甲醇(92∶8)为洗脱溶液,浓缩定容后,用Waters ACQUITY UPLC BEH C18(50 mm×2.1 mm,1.7μm)色谱柱分离,流速0.3 m L/min,以水-甲醇为流动相梯度洗脱,于UPLC-MS/MS仪多反应监测(MRM)模式测定,基质匹配标准溶液外标法定量。结果表明,5种植物生长调节剂在5~500 ng/m L浓度范围内呈良好的线性关系,相关系数(r2)为0.996 1~0.999 6。在0.004,0.02,0.1 mg/kg加标水平下,方法的回收率为75.6%~110.5%,相对标准偏差(RSD)为1.2%~12.8%,方法检出限(LOD,S/N≥3)为0.001~0.002 mg/kg,定量下限(LOQ,S/N≥10)为0.003~0.006 mg/kg。该方法操作简便、灵敏度高、准确可靠,适用于水果中5种植物生长调节剂残留量的同时测定。     

固相萃取/~(18)O标记高氯酸根稀释高效液相色谱-串联质谱法测定水果中的高氯酸盐

建立了水果中高氯酸盐的高效液相色谱-串联质谱分析检测方法。样品采用1%乙酸提取,C18固相萃取柱净化,Waters IC-Pak Anion HR(4.6 mm×75 mm)色谱柱洗脱,流动相为乙腈-100 mmol/L乙酸铵溶液(体积比60∶40),流速0.7 m L/min;液相色谱-三重四极杆质谱联用技术-电喷雾负离子监测模式检测,采用18O标记高氯酸根离子作为内标进行基质校正,内标法定量。结果表明:高氯酸盐在0.1~10.0μg/L范围内线性关系良好,定量下限为1.0μg/kg;在1.0,2.0,10μg/kg 3个加标水平下的回收率为92.5%~110%,相对标准偏差(RSD)为1.4%~5.4%。实际样品检测表明该方法准确可靠,适合于水果中高氯酸盐的测定。