高效液相色谱法同时测定雪上一枝蒿中6种乌头属生物碱含量

建立高效液相色谱法同时测定雪上一枝蒿中苯甲酰新乌头原碱、苯甲酰次乌头原碱、苯甲酰乌头原碱、新乌头碱、次乌头碱、乌头碱等6种乌头属生物碱的含量。采用Thermo Acclaim 120 C_(18)色谱柱,以乙腈:四氢呋喃(25:15)和0.1 mol·L~(-1)醋酸铵溶液(每1000 mL加冰醋酸0.5 mL)为流动相,进行梯度洗脱;流速1.0 mL·min~(-1);柱温30℃;检测波长235 nm。结果显示,6个成分分离度良好,平均回收率为93.26%～102.03%,RSD为0.23%～2.87%。该方法简便准确,重复性好,适用于雪上一枝蒿的质量控制与评价。     

新疆白喉乌头中4种生物碱的分离鉴定及含量测定

采用硅胶柱层析、硅胶柱色谱法等手段对白喉乌头的95%乙醇提取物中的化学成分进行了分离纯化,通过¹HNMR、¹³CNMR对分离得到的4种生物碱的结构进行了鉴定,并采用HPLC法同时测定了其含量。结果表明,从白喉乌头的95%乙醇提取物中共分离得到4个二萜生物碱,分别鉴定为：8-去氧刺乌头碱、异刺乌头碱、高乌甲素、冉乌头碱,其中异刺乌头碱为首次从白喉乌头中分离得到;3批白喉乌头药材中8-去氧刺乌头碱、异刺乌头碱、高乌甲素、冉乌头碱的平均含量分别为0.026 mg·g^-1、0.124 mg·g^-1、1.143 mg·g^-1、0.561 mg·g^-1,其中高乌甲素的含量最高。     

高效液相色谱法测定追风活血膏中8种成分

建立了高效液相色谱(HPLC)测定追风活血膏中士的宁、乌头碱、马钱子碱、当归、乳香、没药、蜕皮甾酮和青藤碱8种成分含量的方法。色谱柱为Agilent ZORBAXSB-C₁₈柱(4.6 mm×250 mm, 5μm);流动相：甲醇(A相),0.1%H₃PO₄水溶液(B相);流速1.0 mL/min;柱温室温;检测波长256 nm。结果显示,8种成分能够达到良好分离,在各自线性范围内线性关系良好,相关系数r均大于0.999;平均加样回收率在98.74%～99.67%之间,相对标准偏差(RSD)在0.85%～1.76%范围内。5批次样品中士的宁、乌头碱、马钱子碱、当归、乳香、没药、蜕皮甾酮和青藤碱的含量分别为0.031～0.349,0.021～0.166,0.024～0.298,0.021～0.219,0.017～0.186,0.015～0.158,0.015～0.149,0.016～0.179 mg/g。本文所建立的HPLC法操作简单、稳定可控,可用于追风活血膏的质量控制。     

抗衰老保健食品中白藜芦醇和辅酶Q10的含量测定

建立了同时测定抗衰老保健食品中白藜芦醇和辅酶Q10的含量的HPLC方法。采用Welch materials C18液相色谱柱,甲醇∶异丙醇(55∶45)为流动相,流速设定为1 mL·min-1,检测波长为PDA定时波长(0.00,306.0)(6.00,306.0)(6.01,275.0)(20.00,275.0),实现了白藜芦醇和辅酶Q10的良好分离分析。白藜芦醇的线性范围为0.52～156.00μg·mL-1,r=0.9999;辅酶Q10的线性范围为0.49～195.52μg.mL-1,r=0.9999。平均加标回收率及RSD分别为97.70%(RSD 0.6%)和97.40%(RSD 0.4%)。本方法灵敏度高、选择性好、操作简单,可方便地用于检测抗衰老类保健食品中白藜芦醇和辅酶Q10的含量。     

高效液相色谱法测定保健食品中葛根素的含量

用高效液相色谱法测定保健食品中葛根素含量,采用DiamonsilTM C18 5μ 4.6 mm×250 mm色谱柱,甲醇∶水=30∶70(v/v;用磷酸调节pH＝3.0)为流动相,检测波长为250 nm.结果为:线性范围3～300 ng(r=0.999993),平均回收率为99.7%,相对标准偏差为1.5%.本法灵敏、快速,结果可靠,可用于保健产品质量控制.     

超高效液相色谱-串联质谱法测定化妆品中粉防己碱、防己诺林碱及马兜铃酸A

采用超高效液相色谱-串联质谱（UPLC-MS/MS）检测技术,建立了化妆品中粉防己碱、防己诺林碱及马兜铃酸A的检测方法。样品经甲醇提取,经流动相（水-甲醇）提取过滤后,采用C18柱（100 mm×2.1 mm×3.0μm）进行分离。结果表明,3种成分在9～176 ng/mL范围内线性关系良好,相关系数大于0.998;加标回收率为85%～115%,相对标准偏差（RSD）小于5%(n=6),检出限均低于0.02μg/g。该方法简单、快速、灵敏,能够满足化妆品中粉防己碱、防己诺林碱及马兜铃酸A的检测需求。     

RP-HPLC-ELSD同时测定附子地上部分中新乌头碱和次乌头碱的含量

采用反相高效液相色谱-蒸发光散射监测器(RP-HPLC-ELSD)测定附子地上部分中新乌头碱和次乌头碱的含量。色谱柱为Krom asil C18(150 mm×4.6 mm,5μm),流动相为乙腈-0.1%乙二胺水溶液(体积比为60∶40),柱温为室温,流速1 mL/m in,漂移管温度89.0℃,气体流量2.60 L/m in。结果表明,新乌头碱和次乌头碱均得到较好分离,均在12.5~400μg/mL呈现良好的线性关系;平均加样回收率分别为100.01%(RSD=0.31%),99.53%(RSD=0.51%)。RP-HPLC-ELSD法具有准确度高,简便快捷,干扰少,重现性好的优点,可用于附子地上部分中双酯型生物碱的测定。     

HPLC法测定白茅根中绿原酸的含量

目的:建立测定白茅根中绿原酸含量的高效液相色谱法。方法:采用高效液相色谱法,C18色谱柱(250×4.6nm,5μm);流动相:甲醇-0.1%磷酸溶液(89:11),检测波长:327nm,流速:1ml/min。结果:绿原酸的平均回收率为90.8,RSD为1.60(n=6),结论:此方法灵敏,专属性好,重现性好。     

高效液相色谱法测定保健食品中20种雌性激素

建立高效液相色谱法同时测定保健食品中20种雌性激素的含量测定方法。样品用甲醇超声提取后,经Oasis?HLB固相萃取柱净化,甲醇洗脱,以高效液相色谱仪定量分析。20种雌性激素均得到较好的分离度,质量浓度与峰面积呈良好的线性关系,相关系数均大于0.995,方法检出限为0.02～0.10μg/mL。3个不同浓度加标水平下,平均回收率为71.9%～112.4%,重复性测定结果的相对标准偏差均小于5.0%。该方法操作简便,定性可靠,定量准确,灵敏度高,适用于保健食品中非法添加雌性激素的检测分析。     

心宝丸中不同产地附子的毒效成分含量测定方法及质量评价

目的：建立心宝丸中附子组分单酯型生物碱和双酯型生物碱毒效成分的含量测定方法，以对不同产地附子制备的心宝丸进行质量评价，优选附子产地。方法：采用HPLC法，使用Phenomenex Gemini C18色谱柱(250 mm×4.6 mm,5μm)，以乙腈-四氢呋喃(25∶15)为流动相A，以0.03 mol/L磷酸二氢钾的0.1%磷酸溶液为流动相B，梯度洗脱，检测波长为232 nm；流速为1.0 mL/min；柱温为25℃。结果：乌头碱、次乌头碱、新乌头碱、苯甲酰新乌头原碱、苯甲酰乌头原碱和苯甲酰次乌头原碱分别在3.2500～25.9997μg/mL、3.0660～24.5280μg/mL、3.2397～25.9179μg/mL、3.7107～18.5083μg/mL、3.9164～19.5822μg/mL、3.8569～19.2845μg/mL范围内线性关系良好；平均回收率分别为99.4%、100.8%、100.6%、100.9%、100.4%和99.4%,RSD分别为1.4%、0.6%、0.6%、1.3%、1.3%和0.7%(n=9);4个不同产地附子制备得到的心宝丸成品中，四川江油...     

Preparation and evaluation of aconitine imprinted microspheres and its application to body fluid samples

To extract aconitine from body fluid samples, aconitine‐molecularly imprinted polymer microspheres with the optimum molar ratios of template/monomer/cross‐linker (1:8:40) as selective sorbents were synthesized by precipitation polymerization. Excellent retention of aconitine on the molecularly imprinted microspheres (MIMs) cartridge was achieved by optimizing the MISPE process, and the binding capacity reached 0.802mg/g, yielding an imprinting factor of 4.76. The MIMs also showed high selectivity for aconitum alkaloids, but not for other kinds of poisonous alkaloids. High recoveries (>89%) for aconitine, hypaconitine, and mesaconitine were got in spiked serum samples. The working curves show linear dependence on aconitine concentration in the range of 2.0–0.1 µg/mL, and the detection limits of aconitine, hypaconitine, and mesaconitine were 16.7, 18.3, 10.2 ng mL^–1, respectively. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

气相色谱法测定保健食品中敌敌畏农药残留

建立了采用气相色谱测定保健食品中敌敌畏农药残留的方法,样品经丙酮提取,二氯甲烷萃取,DB-5弹性石英毛细管柱分离,氮磷检测器检测。方法的线性相关系数为0.999 4,检出限为4.6μg/kg,平均添加回收率在86.1%~95.8%之间,变异系数在4.5%~7.8%之间。测定的16批保健食品均未检出敌敌畏农药残留。     

乌头碱的热解及半衰期研究

采用微量热技术及热重法，结合液质联用技术，探讨了乌头碱的热降解机理、水解机理的热效应等，求出乌头碱的半衰期。结果表明，乌头碱在空气氛围中不稳定，碱性溶液中易水解t_1/2=0.973 h。空气环境中热分解分3步，其分解温度区间分别为185～213℃，248～468℃和484～579℃。相应的反应级数分别为n=1/4、n=4、n=2。对应的活化能分别是154.53，100.97和120.08 kJ·mol^-1。乌头碱应尽可能储存于低温干燥并隔绝空气的环境中。     

不同源性食品性激素残留的检测方法浅析

食品是人体摄入各种营养物质的来源。各种兽药、饲料添加剂在食品原料生产中被广泛使用,造成违禁药物特别是激素类物质在不同源性食品中残留。这些激素残留将对人体健康产生影响。因此,建立适用于不同源性食品激素残留检测的方法尤为重要。本文综述了不同源性食品中性激素残留检测的方法,探讨了利用现代分析测试技术检测不同源性食品中性激素残留方法的发展方向。     

Hospital food handlers in Niterói, RJ, Brazil: intestinal parasitism

A survey for intestinal parasites was carried out with food handlers from two private and three public hospitals in Niterói City, RJ, Brazil. The aim of this research was to verify the enteroparasites prevalence in this professional group. The investigation was divided in two phases. The first phase consisted of interviews with the participants; coproparasitological exams using Lutz, Faust et al. and Baermann techniques; under fingernail material analysis, using Mello et al. modified method; and educational lectures to food handlers. In the second phase, coproparasitological exams were repeated. Positive results were observed in 14.2% (17/120) and 17.1% (12/70) of the individuals in the first and second phases respectively. The most frequent parasite was Entamoeba coli, detected in 48.5% (16/33) of the samples with positive results. Under fingernail residues were observed in 19.2% (23/120) of the food handlers. E. coli cysts were found in one fingernail residue, likewise they were detected in the feces of the same food handler. Such data showed a potential transmission risk of intestinal parasites by food handling, indicating the need of adopting a diagnosis/orientation procedure as a bi-annual routine activity in hospitals, in order to improve the food service quality and population health condition.     

Assessment of the bioactive lipid profiles of oil extracted from Tunisian table olive cultivars (Barouni,Besbassi, and Marsaline cvs.)

Bioactive compounds are components extracted from biological matrices that may offer physiological health benefits and have nutritive value. The present study characterized bioactive lipid components such as fatty acids, phytosterols, policosanol, and triterpenes from table olives. The table olives were processed according to the green Spanish-style method. The obtained results indicate that phytosterol fraction constitutes the major portion of the total unsaponifiable matter. The analysis of phytosterols showed the presence of 11 compounds, β-sitosterol the predominant one. The policosanol composition indicated that hexacosanol, tetracosanol, octacosanol, and docosanol were the main compounds, accounting for over 85% of total policosanols. Pentacyclic triterpenes (cycloartenol and 24-methylene cycloartenol) were found at a higher level (over 85%) compared to tetracyclic triterpenes (β-amyrin, δ-amyrin). These findings reveal that processed table olives contain an interesting amount of various bioactive compounds compared to marine and other floral biological matrices. Thus, processed table olives represent an interesting natural functional food that presents high stability and bioavailability of their natural bioactive ingredients. Practical Applications: Nowadays, with health food gaining popularity among consumers, the demand for natural bioactive compounds and functional food is expanding considerably all over the world. This study focuses on analyzing bioactive lipid components from processed table olives. Fruits were processed according to the green Spanish-style method. The salt content of the brine was adjusted to the minimum sodium chloride value required by the Codex Alimentarius Comission, which is 5%, taking into consideration people suffering from hypertension. This concentration is considered the minimum amount of salt necessary to exhibit antibacterial activities. Considering the results obtained, processed table olives present one of the most valuable potential resources for bioactive lipid compounds and have a considerable ability to preserve the stability of their lipid components. Thus, the food industry in Mediterranean countries can promote processed table olives as conventional functional food with no need for any enrichment or fortification.     

双孢蘑菇粗多糖卫生质量标准的制定

文章主要对双孢蘑菇粗多糖的感官指标、理化指标、微生物指标中的各要素进行检测。分析实际测定数据,参考有关制品卫生标准,并对检测方法、检验规则、标识、包装、运输及贮存要求作出规定,从而制定出双孢蘑菇粗多糖卫生质量标准。此标准可为以双孢蘑菇为原料,经清洗、热煮、过滤、浓缩、提取、超滤、冻干、粉碎等工序制成的可直接稀释食用的干制品提供参考依据。     

HPLC—DAD法测定食品样品中的硫酸软骨素

应用反相液相色谱法测试硫酸软骨素,方法简便快速,易于操作,适合于食品样品的测试,易于在普通的食品实验室推广。该方法在HPLC上的线性范围广,相关系数R〉0．9999,重复性好,有较满意的检出低限。该方法的样品回收率为81．6％-99．3％。     

高效液相色谱在兽药残留中的分析和应用

动物源性食品中的兽药残留是近几年来国际社会开始研究的公共卫生问题之一,而且越来越受到国内外人们的普遍重视。目前就动物源性食品中兽药残留检测方法的研究来说,高效液相色谱法是十分有效的方法之一。本文综述了高效液相色谱在链霉素、氯霉素、四环素、磺胺类药物残留中的分析和应用。     

气相色谱-质谱联用法测定食品中邻苯二甲酸酯类化合物

建立了食品中邻苯二甲酸酯类化合物的气相色谱-质谱（Gc—Ms）测定方法。以乙酸乙酯和环己烷为萃取溶剂,用溶剂萃取食品中的邻苯二甲酸酯类化合物,采用气相色谱-质谱（GC-MS）进行检测。邻苯二甲酸酯的线性相关系数r〉0．999,对实际加标样品的回收率在85％-115％之间,相对标准偏差（1KSD）在1．6％-8．2％之间,适合于食品中邻苯二甲酸酯类化合物的测定。