高效液相色谱法测定烟草中的淀粉含量

研究了用高效液相色谱法测定烟草中的淀粉含量,即先用酸将烟草中的淀粉水解为葡萄糖,再以甘露醇为内标物,用WatersSugar Pak1钙型阳离子交换柱为固定相,0 05g/LEDTA钙钠水溶液为流动相,示差折光仪为检测器测定淀粉水解产生的葡萄糖含量,由葡萄糖含量换算为淀粉含量。该方法的检测限为1 0mg/L,相对标准偏差为1 6%～2 1%,标准回收率在95%～105%之间。并用该方法测定了几种烟草样品中的淀粉含量。     

High Performance Liquid Chromatographic Determination of Phytic Acid in Foods

Phytic acid was quantified using a tetrabutylammonium-formate ion pair on an octadecyl column in HPLC. Unlike previous methods, phytic acid eluted significantly later than the dead volume. Good separations were possible with a linear response up to 40 micrograms and a sensitivity of 0.002 micrograms phytic acid. Results with this method are compatible with conventional methods for phytic acid.     

High Performance Liquid Chromatographic Determination of Agaritine in Cultivated Mushrooms

A sensitive, high performance liquid chromatographic method is described for quantification of agartine, a naturally occurring phenylhydrazine derivative isolated from Agaricus bisporus. Freeze-dried mushrooms were extracted with methanol, evaporated to dryness, and the residue resuspended in 0.005N NaH₂PO₄, pH 4.25 and subsequently passed through a C₁₈ reverse-phase SepPak. A mobile phase of 0.005N NaH₂PO₄, pH 4.25, was pumped through a Partisil SCX (25 cm × 4.6 mm i.d.) cation-exchange column at 0.6 ml/min. Agaritine was monitored at 237 nm and linear standard curves were observed over the range 0–2 μg. Recoveries of agaritine standards averaged greater than 90% while the lower limit of detectability was 0.006 μg. Co-chromatography and UV scans indicated that agaritine from mushroom extracts is the major component absorbing at 237 nm at the retention volume of authentic agaritine.     

高效液相色谱法检测熟制猪肉中呈味核苷酸

以市场上2 款黑猪（HZ1、 HZ2）和2 款白猪（BZ1、BZ2）通脊肉和五花肉为研究对象,对比分析其熟制后肉和汤中5’-肌苷酸、5’-腺苷酸、5’-鸟苷酸、肌苷和次黄嘌呤的含量差异。结果表明：猪肉中5’-肌苷酸含量明显高于其他核苷酸,且五花肉中呈味核苷酸含量远低于通脊肉;白猪肉和汤中5’-肌苷酸含量均显著高于黑猪肉（P＜0.05）,肌苷与次黄嘌呤含量总体上低于黑猪肉,白猪BZ1通脊肉和BZ2五花肉汤中5’-腺苷酸含量最高,白猪BZ2通脊肉5’-鸟苷酸含量最高,黑猪HZ1五花肉5’-鸟苷酸含量最低。综上,白猪肉在鲜味呈现上比黑猪肉更具优势,白猪BZ1最佳,黑猪HZ1最差。     

High Performance Liquid Chromatographic Determination of Vitamin C in Fresh Tomatoes

A reverse phase ion-pairing HPLC method for determining vitamin C in fresh tomatoes was developed. An internal standard was used for calibration and quantitation. Recoveries of vitamin C from fresh tomato samples that had been spiked with known amounts of the acid ranged from 96 to 105%. Determination of the vitamin C in fresh tomatoes by this method compared favorably with similar analyses using the standard indophenol titration method.     

High Performance Liquid Chromatographic Determination of Organic Acids in Dairy Products

A simple isocratic HPLC technique was developed for the quantitative analysis of organic acids in dairy products. An Ammex HPX- 87 column at 65°C, 0.0090N H₂SO₄ mobile phase and UV detection at 220 and 275 nm were utilized. Orotic, citric, pyruvic, lactic, uric, formic, acetic, propionic, butyric, and hippuric acids were quantitated for whole milk, skim powder, cultured buttermilk, sour cream, cottage cheese, yogurt, sharp Cheddar cheese, and blue cheese. Over 90% recoveries of acids added to whole milk were observed for ail acids except butyrid; the average recovery for butyric was 86%.     

高效液相色谱法测定蔬菜中氨基甲酸酯类农药

建立高效液相色谱-柱后衍生测定蔬菜中6种氨基甲酸酯类农药残留的方法。样品中的氨基甲酸酯类农药经乙腈溶剂超声提取后,CARB/NH_2固相萃取柱净化,高效液相色谱-柱后衍生法进行定量分析。结果表明在一定浓度范围内质量浓度与峰面积有良好的线性关系,其线性相关系数为0.999 2~0.999 8,加标回收率在79%~91%之间,相对标准偏差(RSD)为0.8%~4.9%,方法检出限为0.002 mg/kg~0.005 mg/kg。     

高效液相色谱法测定甲鱼油中EPA、DHA的含量

建立分离检测广西黄沙鳖甲鱼油中的EPA和DHA的高效液相色谱法。试验采用岛津VP-ODS色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇和水(体积比70∶30),紫外检测波长为254 nm,流速为0.7 mL/min,柱温为30℃。甲鱼油经0.5 mol/L KOH-乙醇溶液进行皂化,三乙胺-溴苯乙酮酯化后直接上机分析。结果表明:EPA、DHA在0.025 mg/mL~0.15 mg/mL范围内线性关系良好,R2EPA为0.999 1、R2DHA为0.999 5;该法用于甲鱼油的检测,回收率EPA为96.00%～98.67%,DHA为92.00%～98.00%,该法简便、快速、重现性好。     

高效液相色谱法测定乳糖酶水解产物中的糖类

用高效液相色谱法测定了乳糖酶水解产物中的糖类 ,以水为流动相 ,用Sugar pakI(Waters)色谱柱和示差折光检测器 ,一次进样同时分离出样品中的半乳糖、葡萄糖、乳糖、低聚糖。测定了半乳糖、葡萄糖、乳糖的含量 ,线性相关系数 0 9991～ 0 9997,变异系数 0 87%～ 1 2 % ,回收率 96 73%～ 10 2 6 %。     

高效液相色谱法检测鸡蛋中四种激素残留量

建立一个简便、重现性好测定鸡蛋中的雌二醇、雌酮、雌三醇及睾酮残留量的方法。使用高效液相色谱法,选择流动相为:乙腈∶甲醇∶四氢呋喃∶(0.01 mol/l)醋酸钠=2∶2∶1∶5,能够有效提高色谱峰的分离度,190 nm~800 nm波段下扫描,选择270 nm为最佳吸收波长,柱温:30℃。结果表明4种激素的方法检出限为0.06 mg/kg~0.17 mg/kg,样品回收率是79.23%~102.26%,相对标准偏差为1.05%~4.21%。该方法准确度高,操作简便。     

反相高效液相色谱法测定雪莲果叶中的绿原酸

采用反相高效液相色谱法对雪莲果叶中的有效成分绿原酸进行分离,并对其含量进行测定,建立反相高效液相色谱法测定雪莲果叶中绿原酸含量的方法。色谱柱为Hypersil ODS-2 C18 柱(4.6mm × 300mm,5μm),流动相为乙腈- 体积分数0.5% 磷酸溶液(8:92,V/V),流速为1.0mL/min,检测波长为325nm,柱温为25℃。绿原酸在10～100μg/mL 范围内呈良好线性关系,相关系数为0.9999,加标回收率为97.0%,RSD 为1.10%。本法快速、简单、准确、分离度好,可用于实际样品的检测。     

高效液相色谱法测定蔬菜中8种氨基甲酸酯类农药残留

建立了固相萃取.高效液相色谱柱后衍生荧光检测蔬菜中涕灭威亚砜,涕灭威砜,灭多威,三羟基克百威,涕灭威,克百威,甲萘威及异丙威等8种氨基甲酸脂类农药残留的分析方法.本文对测定氨基甲酸酯农药残留的分离条件,提取溶剂,洗脱溶剂,净化材料和基质效应进行了优化试验.结果显示,8种氨基甲酸脂类农药在0.1～1.0 mg/L的浓度范...     

高效液相色谱法快速测定酱腌菜中的姜黄素

为探讨用高效液相色谱法快速测定酱腌菜中姜黄素的方法,对提取条件、提取方法、流动相等进行优化实验。结果表明：采用ZORBAX SB C18(150mm × 4.6mm,5 μ m)分析柱,磷酸溶液(pH2.5)- 乙腈(50:50,V/V)为流动相,420nm 的检测波长可以达到理想的分离效果和满意的检出限;该法重复性好,定量检出限为1.5mg/kg、线性范围为1.5～2900.0mg/kg、加标回收率均在95%～108% 之间、相对标准偏差均在0.9%～1.6%(n=5)之间。超声提取法和保温振荡浸提法是提取酱腌菜中姜黄素的简单高效的方法。     

A Simple Liquid Chromatographic Method for Determination of B6 Vitamers in Raw and Cooked Chicken

Four forms of vitamin B₆ (B₆ vitamers) in various chicken tissues were determined by a liquid chromatographic method. The vitamers were extracted from the tissues with metaphosphoric acid and separated on a C₁₈ reverse phase column followed by fluorescence detection. Recoveries of added vitamins at two concentrations were mostly between 84.5% and 107.9% The most abundant form of B₆ in raw tissues was pyridoxal phosphate (PLP) followed by pyridoxamine phosphate (PMP). Cooked tissues contained more PMP than PLP. The levels of pyridoxal (PL) and pyridoxamine (PM) were relatively low. Data also indicated a net increase of PMP and PM vs a decrease of PLP and PL during cooking.     

高效液相色谱-质谱法测定蔬菜中矮壮素残留

为建立蔬菜中矮壮素残留的高效液相色谱- 电喷雾离子阱质谱(LC-ESI/MS)的检测方法,样品中的矮壮素残留采用甲醇- 水- 乙酸溶液提取,离心,分取部分上清液过SCX 阳离子交换固体萃取小柱,LC-ESI/MS 法测定,以保留时间和特征离子定性、外标法定量。结果表明,矮壮素在0.03～10mg/L 范围内线性良好,线性相关系数为R2=0.9991,加标回收率为74.92%～103.28%,相对标准偏差为2.92%～10.48%,方法定量下限可达0.02mg/kg。     

柱前衍生-高效液相色谱法测定暗纹东方鲀肉中牛磺酸含量

运用柱前衍生-高效液相色谱法测定暗纹东方鲀肉中牛磺酸的含量,以邻苯二甲醛为衍生剂,样品液与衍生剂进行衍生反应的体积比为1∶1,反应时间为1 min,甲醇-乙腈-水(体积比10∶20∶70)为流动相,采用XbridgeTMC18色谱柱,波长为330 nm,流速1 mL/min,进样量20μL的条件下检测样品中的牛磺酸。结果表明:牛磺酸的线性范围为5～30μg/mL,相关系数R2为0.999 1,回收率范围95.35%～98.19%,变异系数(RSD)=2.03%～3.71%(n=3),样品6次重复测定的RSD=0.51%,最小检出限1.14μg/mL。     

A High Performance Liquid Chromatographic Method for Chlorogenic Acid Determination in Sunflower Seeds

A new high performance liquid chromatographic (HPLC) method for chlorogenic acid determination in sunflower seeds is described. This method offers a relatively rapid and highly selective way to separate chlorogenic acid from caffeic acid and other polyphenolic compounds in sunflower seeds. The HPLC method results are compared with those of the spectrophotometric method and no significant difference is shown between methods using confectionery seeds but significant differences are shown with the oilseed varieties.     

高效液相色谱法测定蔬菜水果中七种植物激素的残留量

建立高效液相色谱法测定果蔬中7 种植物激素残留的方法。选择10 种果蔬样品,经体积分数80% 甲醇提取后、过C18 柱净化,用带有紫外检测器的液相色谱仪测定,外标法定量。通过对该方法的精密度和加标回收实验,所有激素的添加回收率均在70.23%～98.10% 之间,回收率的变异系数在3.34%～10.12% 之间,方法的最低检出限为0.004～0.02mg/kg、最低定量限为0.01～0.1mg/kg,所建立的果蔬中植物激素残留量的测定方法满足国家标准对食品中农药残留测定的要求,可提供给相关部门用于对相关农产品、食品的质量监控。     

RP-HPLC快速检测牛奶中7中四环素类药物残留量的研究

目的：建立快速检测牛奶中7 种四环素类药物残留的反相高效液相色谱法。方法：用0.1mol/L McIlvaine-EDTA 溶液和50% 三氯乙酸(TCA)溶液共同处理牛奶样品,通过Waters Oasis HLB 固相萃取柱进行净化处理。仪器条件中所用色谱柱为SunfireTM C18(250mm × 4.6mm,5μm)柱,以甲醇- 乙腈-0.01mol/L 草酸(pH2)为流动相,采用梯度洗脱模式。结果：7 种四环素类药物线性范围宽,峰面积和样品浓度在0.05～1μg/ml 范围内呈很好的线性关系,加标平均回收率为78.66%～106%,最低检测限为0.02μg/ml。结论：该方法操作简单、重现性好、检测限低、灵敏可靠,可在14min 内同时将四环素等7 种四环素类药物达到基线分离。     

应用反相高效液相色谱法测定保健品中的腺苷

本文应用反相高效液相色谱线性梯度洗脱法对保健品中的腺苷进行分离腺苷测定。样品经充分粉碎后,准确称量(其中腺苷含量范围为0.25～0.1mg),加适量水,在超声波振荡器中萃取80min,经离心机离心,吸取上层清液,用0.45μm微孔滤膜过滤;用Lichrospher100 RP-C18柱,pH4.5～5.5的磷酸二氢钾溶液和甲醇作流动相,在1.0mL/min的流速和线性梯度洗脱下,能将腺苷完全分离,在波长260nm处,应用外标法定量。其标准曲线在(1～10)ug/mL的浓度范围内线性良好,其相关系数为1.000;6次重复变异系数为1.59％,加标回收率在103％～105％之间。