蜂胶提取物在大鼠体内组织分布研究

研究蜂胶提取物在大鼠体内的组织分布规律。蜂胶提取物以1.8g/kg大鼠灌胃给药后,用HPLC-UV法测定心、肝、脾、肺、肾中咖啡酸,香豆酸,阿魏酸,异阿魏酸和3,4-二甲氧基肉桂酸的含量。色谱柱Zorbax Extend-C18(250 mm×4.6 mm,5μm),流动相为(A)甲醇-(B)0.2%(φ(HAC))冰醋酸水溶液梯度洗脱;柱温:35℃;检测波长:320nm;进样量:10μL;流速:1.0mL/min。建立了五种酚酸类成分在大鼠心、肝、脾、肺、肾中的HPLC含量测定方法。该方法简便、快速、重复性好,适用于大鼠灌胃蜂胶提取物后,酚酸类成分的体内组织分布研究。     

土壤中氨基甲酸酯类农药检测的方法优化

为高效准确地测定土壤中10种氨基甲酸酯类农药，研究建立一种适用于土壤中10种氨基甲酸酯类农药含量的柱后衍生-液相色谱快速检测方法。试验优化提取条件、固相萃取柱和色谱条件，结果表明：水浴温度35℃,提取液为V(甲醇)∶V(二氯甲烷)=1∶1,提取体积为50 mL、超声时间25 min,采用Carb/NH₂固相萃取柱净化，选择Shim-pack FC-ODS(75 mm×4.6 mm, 3μm)液相色谱柱分析测试。本检测方法的线性系数均可达到0.999 3以上；线性范围为0.02～10μg/mL;检出限均小于2.0μg/kg;对10.0 g左右的土壤进行低(5μg/kg)、中(50μg/kg)、高(500μg/kg)三个浓度水平的加标测试时，10种氨基甲酸酯类农药的加标回收率为75.7%～118.5%;重现性良好，相对标准偏差为0.8%～6.8%;该方法能够满足测定土壤中10种氨基甲酸酯类农药的需要。     

高效液相色谱-串联质谱同时测定蜂胶中氯霉素、甲砜霉素和氟甲砜霉素残留量

建立了高效液相色谱-串联质谱同时测定蜂胶中氯霉素、甲砜霉素和氟甲砜霉素残留的方法。结果表明:在1~30μg/L范围内氯霉素、甲砜霉素和氟甲砜霉素3种目标物的线性关系良好,相关系数R~2均大于0.997;氯霉素的检出限为0.01μg/kg,甲砜霉素和氟甲砜霉素的检出限均为0.05μg/kg;3种目标物的加标回收率为67.3%~121%、变异系数为0.82%~12.2%。该方法准确可靠、灵敏简便,能够满足对蜂胶中氯霉素类药物的残留确证。     

高效液相色谱法测定牙膏中叶绿素铜钠盐的含量

在酸性条件下,以聚酰胺粉吸附牙膏中叶绿素铜钠盐,解吸附洗脱,经YMC Carotenoid C30 (4.6 mm×250 mm,3 µm)色谱柱分离,光二极管阵列检测器(PDA)检测,建立了高效液相色谱法测定牙膏中叶绿素铜钠盐含量的方法。样品经甲醇-叔丁基甲醚-0.5%醋酸混合溶液为流动相进行梯度洗脱,流速1.0 mL/min,柱温30 ℃,检测波长405 nm。结果表明,叶绿素a铜钠盐和叶绿素b铜钠盐在5.0~100.0 mg/L质量浓度范围内,具有较好的线性关系,相关系数分别为0.999 8和0.999 7;检出限均为1.5 μg/kg,定量限均为5.0 μg/kg;加标回收率为87.2%~97.8%,RSD为1.7%~2.9%。     

GPC-HPLC-MS/MS法测定饲料中20种磺酰脲类除草剂

以饲料为实验材料,建立了测定饲料中20种磺酰脲类除草剂含量的凝胶渗透色谱-液相色谱串联质谱(GPC-LC-MS/MS)法。样品经凝胶渗透色谱净化后,采用液相色谱串联质谱法(HPLC-ESI-MS/MS)分析,多反应监测模式下(MRM)外标法定量。结果表明,20种磺酰脲类除草剂在1～20μg/L范围内相关系数≥0.995,线性关系良好;检出限均为0.5～1.0μg/kg。该方法在1～10μg/kg添加水平下,相对标准偏差均<10%,回收率为71.2%～112.4%。     

超高效液相色谱-串联质谱法测定牛肉中的阿托品

建立了超高效液相色谱-串联质谱法测定牛肉中阿托品残留量的分析方法。样品用0.1 mol/L磷酸二氢钾缓冲溶液-乙腈(4∶1)提取,采用Agilent Zorbax Eclipse Plus C18柱(4.6 mm×50 mm,2.7μm)为分离柱,以乙腈和0.1%甲酸水作为流动相,梯度洗脱。在电喷雾正离子模式下(ESI+),用多重反应监测(MRM)模式进行检测,基质匹配外标法定量。在优化的实验条件下,阿托品的检出限为0.5μg/kg,定量限为1.5μg/kg,线性范围为0.10～5.0 ng/mL,相关系数r≥0.999。在1.0、5.0和10μg/kg这3个加标水平下,阿托品的平均回收率为89.5%～95.2%,相对标准偏差(RSD_6)为2.07%～5.03%。该方法简单、灵敏度高、结果准确可靠,可用于牛肉中阿托品残留量的测定。     

气相色谱-质谱联用仪测定蜂胶中的多环芳烃

蜂胶中的多环芳烃用乙腈提取后再用正己烷萃取,经固相萃取柱净化,浓缩定容后,用气相色谱-三重四极杆串联质谱联用仪进行测定,以外标法定量检测蜂胶中多环芳烃的残留量.该方法的线性范围为1～100μg/L,相关系数均大于0.99,回收率均在70.0％ ～95％,相对标准偏差均在1.0％ ～5.0％,表明该方法的准确度和精密度均...     

QuEChERS-超高效液相色谱串联质谱法测定甜菜中15种除草剂

[目的]建立了甜菜中15种除草剂残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。[方法]甜菜样品用乙腈提取,经QuEChERS方法净化后,在超高效液相色谱-串联质谱仪电喷雾正负离子在线切换多反应监测(MRM)模式下测定,外标法定量。[结果]15种除草剂在0.1～5.0μg/L范围内呈良好的线性关系,相关系数均大于0.996,检出限(LOD)为0.001～0.038μg/kg,定量限(LOQ)为0.004～0.127μg/kg。1.0、5.0、10.0μg/kg 3个添加水平下15种除草剂回收率范围为82.8%～109.2%,相对标准偏差为0.81%～6.4%。[结论]该方法高效、准确,灵敏度和精密度均满足甜菜多除草剂残留检测的要求。     

高效液相色谱法测定化妆品中苯扎溴铵

建立了化妆品中苯扎溴铵的高效液相色谱分析法。采用φ(甲酸)=0.5%的甲醇溶液超声提取样品,以CAPCELLPAK SCX色谱柱(4.6 mm×150 mm,5μm)分离,流动相为40 mmol/L乙酸铵水溶液(含φ=0.1%三乙胺,调pH=4.0)和乙腈(梯度洗脱),流速1.0 mL/min,检测波长215 nm,柱温25℃,进样量10μL。该方法的检出限50 mg/kg,线性范围5.0～200.0μg/mL,加标回收率92.4%～97.3%,相对标准偏差为3.41%～6.56%。     

超高效液相色谱串联质谱法测定中药类保健品中6种有毒生物碱

建立了QuEChERS法净化,超高效液相色谱串联三重四极杆质谱法(UPLC-MS/MS)测定中药类保健品中6种有毒生物碱含量的方法。样品以1%甲酸-乙腈超声提取,BEH C18色谱柱(1.7μm, 2.1 mm×100 mm)分离,以0.1%甲酸-2 mmol/L乙酸铵的水溶液与含0.1%甲酸的乙腈溶液为流动相梯度洗脱,三重四极杆质谱正离子多反应监测模式检测(MRM),外标法定量。在优化的色谱质谱条件下,6种生物碱在浓度0～20 ng/mL范围内与峰面积线性关系良好,相关系数均大于0.994 2。方法检出限(LOD,S/N=3)为0.002～0.05μg/kg,定量限(LOQ,S/N=10)为0.007～0.15μg/kg,在20、50、100μg/kg的加标浓度下,6种目标分析物的平均回收率为62.3%～98.2%,相对标准偏差(RSD)为1.6%～3.6%。该方法准确、高效、简便,适用于中药类保健品中有毒生物碱的定性、定量筛查。     

蜂胶香皂中黄酮成分的测定

采用分光光度比色法测定蜂胶中的总黄酮含量。使用无水乙醇萃取蜂胶香皂中的黄酮成分,用硝酸铝作为显色剂,在415 nm处进行比色,与标准曲线相对比进行定量计算。本方法最低可以测定总黄酮含量在0.06%的蜂胶香皂样品。     

蜂胶的抑菌性能及其在牙膏中的应用研究

口腔疾病是影响人体健康的常见疾病,大多是由于口腔中的致病菌引起的。通过测定超临界CO2萃取的蜂胶提取物对4种口腔常见致病菌的最小抑菌浓度,证实其具有良好的抑菌性能。将其应用于牙膏,对牙膏作抑菌环试验。结果显示,该牙膏与空白牙膏相比,抑菌效果有显著性差异,与阳性对照牙膏相比,抑菌效果相当,说明该牙膏具有良好的抑菌能力。     

树脂法精制蜂胶高生物活性黄酮醇

考察了5种树脂对蜂胶中的水溶性黄酮醇的吸附和洗脱性能。以质量分数为65%的乙醇为提取剂,提取温度为38℃,以质量分数为60%的乙醇洗脱,通过比较吸附量、洗脱率以及所得水溶性黄酮醇的含量,最后得出以V(D4020)∶V(聚酰胺)=2∶1的混合型树脂为最佳选择。采用该种树脂,水溶性黄酮醇的最大吸附量为32.76mg/mL,洗脱率为94.68%,提取率为8.27%。     

Comparison of Antioxidant Activity of Ethanolic Extracts of Propolis Obtained by Different Extraction Methods

The antioxidant activities of the ethanolic extracts of propolis obtained by different extraction methods (high hydrostatic pressure extraction, leaching at room temperature and heat reflux extraction) were investigated in relationship to their total polyphenol and flavonoid contents by two different assays, namely, the β‐carotene bleaching and 1,1‐diphenyl‐2‐picrylhydrazyl (DPPH) free radical scavenging assay systems. The results showed that the ethanolic extracts of propolis obtained by high hydrostatic pressure extraction and leaching at room temperature had relatively strong antioxidant activities, which may be correlated with the total polyphenol and flavonoid contents. Antioxidant activities of ethanolic extracts of propolis obtained by high hydrostatic pressure extraction were the same as those of ethanolic extracts of propolis obtained by leaching at room temperature. Leaching at room temperature usually needs a few days, and can take even more than 7 d, while high hydrostatic pressure extraction needs only 1 min. These findings further illustrate that the high hydrostatic pressure extraction has a bright prospect for extracting flavonoids from propolis.     

不同产地蜂胶中总黄酮的提取及含量测定

目的:测定不同产地蜂胶中总黄酮的含量,为蜂胶的质量控制提供更多依据。方法:通过正交设计试验,优选蜂胶中总黄酮的提取方法;以芦丁为对照品,用分光光度法测定不同产地蜂胶中总黄酮的含量。结果:国内主要产地的蜂胶中总黄酮含量均高于巴西蜂胶,且河南,山东产蜂胶中总黄酮含量大于20%。结论:该方法可靠,测定结果能反映客观实际,可作为蜂胶质量控制指标之一。     

超临界CO_2萃取蜂胶有效成分的研究

采用四因素三水平的正交设计,研究了超临界CO2萃取蜂胶有效成分的萃取工艺,并用色质联用法分析了蜂胶提取物的成分组成。结果表明,超临界CO2萃取蜂胶有效成分最佳工艺条件为:萃取温度55℃、萃取压力30MPa、CO2循环量0 6kg/g、w(携带剂)=5%。通过GC-MS分析,共鉴定出其中24个组分。     

High hydrostatic pressure extraction of flavonoids from propolis

A high hydrostatic pressure extraction (HHPE) method is presented for the extraction of flavonoids from propolis. Various experimental conditions of the HHPE process, such as solvents, ethanol concentration (35–95%, v/v), HHPE pressure (100–600 MPa), HHPE time (1–10 min) and solid/liquid ratio (1:5–1:45 g cm^?3), were investigated to optimize the extraction process. The extraction yield with HHPE for 1 min was higher than those using extraction at room temperature for 7 days and heat reflux extraction for 4 h respectively. From the viewpoints of extraction time, the extraction efficiency and the extraction yield of flavonoids, HHPE was more effective than the conventional extraction methods studied. Copyright © 2004 Society of Chemical Industry     

树脂法富集分离蜂胶总黄酮

实验考察了7种大孔树脂及聚酰胺对蜂胶总黄酮的吸附率和解吸率,结果显示,AB-8树脂对蜂胶总黄酮有较高的吸附解吸能力,适合富集蜂胶总黄酮。实验还对影响AB-8树脂富集蜂胶总黄酮的各因素(吸附时间、吸附温度、解吸温度、洗脱剂乙醇浓度、洗脱剂用量)进行了研究,所得AB-8树脂对蜂胶总黄酮的富集工艺为:35℃水浴静态吸附5 h,75%乙醇7BV洗脱,总黄酮解吸率可达90%,所得蜂胶浸膏总黄酮含量达30%。     

Use of Propolis in the Sanitization of Lettuce

The present study aimed to determine the effectiveness of propolis in reducing the microbial load in ready-to-eat (RTE) and fresh whole head (FWH) lettuces (Lactuca sativa L.) type Batavia. Two sanitizing solutions were employed: sodium hypochlorite (SH) and propolis (PS), during 15 and 30 min. Tap water (TW) was used as a control. Regarding the mean reduction on aerobic mesophiles, psychrotrophic and fecal coliforms, the SH and PS treatments showed the same pattern of variation. In all cases, PS was slightly more effective in the microbiological reduction in comparison with commercial SH. Reductions between two and three log cycles were obtained with PS on aerobic mesophiles and psychrotrophic counts. The information obtained in the present study can be used to evaluate the potential use of propolis as product for sanitizing other vegetables and for developing other food preservation technologies, with impact on human health.     

Kinetics of lipid oxidation in the presence of cinnamic acid derivatives

The effects of seven (prenyl‐ and methoxy‐) derivatives of cinnamic acid (0.1 mM) on the kinetics of lipid (sunflower oil triacylglycerols, TGSO) bulk phase oxidation at 80 °C have been compared. Synthesis of prenyl cinnamic acid derivatives: 3‐prenyl‐4‐hydroxy‐cinnamic acid (PHC), 3,5‐diprenyl‐4‐hydroxy‐cinnamic acid (DPHC), 2,2‐di‐methyl‐6‐carboxy‐ethenyl‐2H‐benzopyran (DMCB), 2,2‐dimethyl‐6‐carboxy‐ethenyl‐8‐prenyl‐2H‐benzopyran (DCEPB) present in Brazilian propolis has been performed. The monoprenyl derivative (PHC) has been found to exert a higher antioxidant activity as compared to the diprenyl derivative (DPHC). However, cinnamic acid derivatives DMCB and DCEPB have caused no change in the kinetics of TGSO oxidation. The results obtained have been compared with those on related compounds containing a cinnamic acid moiety as a structural feature, such as 4‐hydroxy‐cinnamic (p‐coumaric), 3‐methoxy‐4‐hydroxy‐cinnamic (ferulic) and 3,5‐dimethoxy‐4‐hydroxy‐cinnamic (sinapic) acids, as well as with data on butylated hydroxytoluene (BHT) and α‐tocopherol (αToc). PHC has shown a stronger antioxidant efficiency than BHT, p‐coumaric and ferulic acid, but a weaker antioxidant efficiency than α‐Toc and sinapic acid. The observed antioxidant effect of DPHC was stronger than that of p‐coumaric and ferulic acids and weaker than that of α‐Toc, BHT and sinapic acid.