高效液相色谱法测定发酵乳中的乳糖、葡萄糖和半乳糖

利用高效液相色谱法测定发酵乳中乳糖、葡萄糖、半乳糖的含量。样品通过Carrez法处理沉淀蛋白,采用Aminex HPX 87H色谱柱, 5mmol/L H2SO4溶液为流动相,流速0.6mL/min。结果表明：利用该法进行色谱分析各组分达到较好的分离,各糖组分在0.5～12mg/mL范围内呈现良好线性关系,相关系数为0.9986～0.9999(n＝ 5),样品回收率为96.45%～101.78%;精密度实验表明,各组分峰面积RSD在0.62%～4.21%之间(n＝ 5);重现性实验表明,各组分含量测定值RSD为1.86%～3.44%。该法测定样品快速、准确、可靠,为发酵乳贮藏过程中关键糖含量的测定提供参考依据。     

高效离子交换色谱法测定半乳糖、葡萄糖、乳糖及低聚半乳糖含量

建立离子色谱法定量测定以乳糖为原料、使用β-半乳糖苷酶生产的低聚半乳糖产品的方法。样品前处理过程中用体积稀释法代替质量稀释法,采用高效CarboPac PA20阴离子交换色谱柱和积分安培法检测,并对淋洗液组成进行优化。优化后的方法加标回收率90.58%～99.45%,相对标准偏差为3.54%。半乳糖、葡萄糖、乳糖的方法检出限分别为0.24、0.59、0.75 μg/g。半乳糖和葡萄糖在0.2～7 μg/mL、乳糖在0.6～10 μg/mL的范围内,其质量浓度与峰面积线性关系良好,相关系数在0.999 2～0.999 9之间。用此方法测定6 种原料低聚半乳糖,目标组分总含量为95.84%～101.19%。     

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。     

高效阴离子交换色谱法测定生鲜乳中硫氰酸盐的含量

建立高效阴离子交换色谱电导法分析生鲜乳中硫氰酸盐的方法。采用乙酸溶液沉淀生鲜乳中蛋白,过滤后用RP 柱去除样品中的脂类物质。净化后,直接将试样注入离子色谱仪分离,淋洗液OH－浓度为60mmol/L,外标法定量。稳定性实验中5 次进样1mg/L 硫氰酸根溶液的保留时间平均值为15.445min(RSD 为0.12%),峰面积平均值为0.1839μS·min(RSD 为0.26%)。方法回收率为96.0%～98.0%,RSD ＜ 1.06%,检测限为0.2mg/kg,线性范围为0.5～6mg/L。     

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。     

应用高效液相色谱快速测定奶粉中的乳糖,蔗糖,葡萄糖

讨论了应用高效液相色谱（ＨＰＬＣ）对奶粉及调制奶粉中的乳糖,蔗糖,葡萄糖的一种快速测定方法。样品经简单的前处理后由Ｃａｒｂｏｈｙｄｒａｔｅ Ａｎａｌｙｓｉｓ柱分离,流动相为乙腈／水,示差折光检测,奶粉中乳糖,蔗糖,葡萄糖完全分离并定量测定。方法简便,快速,结果令人满意。     

离子色谱法测定奶粉中的葡萄糖、蔗糖和乳糖

建立高效阴离子交换色谱-脉冲安培检测法测定奶粉中葡萄糖、蔗糖和乳糖的方法。以METROSEP CARB 1(150mm×4.0mm)阴离子交换柱为分离柱,脉冲安培检测,37mmol/L NaOH溶液为淋洗液,以柠檬酸作为蛋白质沉淀剂。葡萄糖、蔗糖和乳糖的线性范围分别为1～40、1～50、1～50mg/L,相关系数分别0.9966、0.9968、0.9985,检出限分别为0.014、0.091、0.083mg/L,精密度为1.10%～4.96%,回收率为90.13%～104.83%。该方法分析时间短,前处理简单,适用于快速测定奶粉中的葡萄糖、蔗糖和乳糖。     

高效液相色谱法测定乳粉及液态奶中牛磺酸含量

建立高效液相色谱法测定乳粉和液态奶中牛磺酸含量。样品用水溶解,超声提取10 min,提取液经亚铁氰化钾和乙酸锌沉淀蛋白后,离心,上清液用异硫氰酸苯酯和三乙胺衍生化,室温衍生1 h,加入正己烷为衍生化终止剂,静置分层,下层溶液用水定容后过0.22μm微孔滤膜,过滤液经Diamonsil AAA氨基酸分析柱(4.6×250 mm,5μm)分离,以0.05 mol/L乙酸钠水溶液(pH值=6.50)和甲醇/乙腈(1/1,V:V)为流动相进行梯度洗脱。采用外标法定量,在5.0～40μg/mL线性范围内相关系数(r)大于0.999,线性关系良好,定量限为5 mg/100 g(S/N≥10),添加水平为5、10、25 mg/100 g时,回收率范围在90%～108%之间,相对标准偏差范围为1.16%～2.24%。结果显示,本方法准确、可靠,满足乳粉和液态奶中牛磺酸含量的有效确定,特别对于特膳奶粉比GB方法更适合样品中牛磺酸含量的有效检测。     

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.     

高效液相色谱法测定乳与乳制品中的三聚氰胺

目的建立乳与乳制品中三聚氰胺的测定方法。方法样品用0.1 mol/L的盐酸提取,再用60 g/L的磺基水杨酸沉淀蛋白。缓冲液为10 mmol/L柠檬酸与10 mmol/L辛烷磺酸钠混合溶液,以缓冲液 乙腈(85 15,体积比)为流动相,使用Kromasil KR100-5C8柱,配备有二极管阵列检测器的高效液相色谱仪在200~400 nm范围内对待测组分进行分离和测定。结果样品中三聚氰胺的添加回收率在80%~105%之间,相对标准偏差(RSD,n=6)小于5.24%,方法的定量限为1.0 mg/kg。结论该方法快速、准确,操作简便,能够满足乳与乳制品中三聚氰胺的分析要求。     

Comparison of High Performance Liquid Chromatography and Enzymatic Method for the Measurement of Lactose in Milk

A high performance liquid chromatographic (HPLC) procedure was compared with an enzymatic method for the measurement of lactose in milk. A new rapid HPLC sample preparation technique was used for precipitating milk proteins with 2-propanol. Results indicated that lactose detected in milk (expressed as percentage) was consistently lower with the enzymatic method than the HPLC procedure. Mean difference between the two methods was 0.15% with a range of 0.04 to 0.51. Coefficient of variability for the HPLC and enzymatic methods were 1.02 and 2.75, respectively. Recovery of added lactose in milk by HPLC was 100.3% for whole milk, 97.1% for low fat milk, and 99.5% for skim milk.     

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%.     

High Performance Liquid Chromatographic Determination of Carbohydrates in Raw and Cooked Vegetables

The soluble sugar contents of 17 raw and cooked vegetables were determined by TLC and HPLC. In general, the soluble carbohydrate content of vegetables is low. For raw materials the highest content was found in carrot, red cabbage, egg plant, green bean and leek. Upon cooking the glucose, fructose and total sugar contents decrease and this diminution is more drastic in the case of frying. The amount of sucrose, except in the case of carrot, egg plant and green bean, increases with cooking. The maltose content of the broad bean increases in the culinary process.     

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烟草中的果糖、葡萄糖和蔗糖

以72%(体积比)乙腈/28%水预混合溶液作流动相,High-Performance Carbohydrate卡套柱作色谱柱,等梯度洗脱,采用带示差折光检测器的高效液相色谱仪测定了烟草中的果糖、葡萄糖和蔗糖含量。结果表明:方法的日内精密度和日间精密度的范围分别为0.46%~1.54%和0.96%~4.74%,回收率97.0%~102.3%,果糖、葡萄糖和蔗糖的检出限(LOD)分别为95,107和105μg/mL(S/N=3∶1),可以满足烟草中果糖、葡萄糖和蔗糖含量的日常检测要求。     

HPLC法测定乳饮料中纽甜含量的研究

建立快速、准确测定乳饮料中纽甜含量的高效液相色谱检测方法。样品以20%乙腈水溶液为提取液,硫酸锌和亚铁氰化钾为沉淀剂进行前处理,采用ZORBAX SB-C18(250 mm×4.6 mm,5μm)色谱柱,200 nm检测波长,磷酸氢二铵(0.020 mol/L,pH 3.5~4):乙腈=(70∶30)为流动相进行等度洗脱分离。纽甜在0.2μg/m L~50.0μg/m L范围内线性良好,在0.8 mg/kg~5.0 mg/kg加标范围内,回收率为90.1%~96.1%,RSD值为1.7%~2.1%,最低定量限为0.30 mg/kg。     

高效液相色谱法测定发酵液中的D-核糖与葡萄糖

以RID为检测器,建立高效液相色谱法定量测定发酵液中葡萄糖和D-核糖的方法。该方法的测定条件为:柱型Shodex Suger SH1011,流动相为0.005 mol/L的稀硫酸溶液,柱温为50℃,进样量为10μL。底物葡萄糖和产物D-核糖的出峰时间分别为11.573 min和13.313 min。得到底物葡萄糖和产物D-核糖的回归方程分别为Y=6.868 4X-0.069 1和Y=6.556 5X+0.004 6,其中Y为葡萄糖或D-核糖的质量浓度,X为对应的峰面积。线性范围在2 g/L~45 g/L时,该法精密度、稳定性和重现性均良好;葡萄糖的平均回收率为99.27%,D-核糖的平均回收率为99.61%,RSD值分别为0.38%和0.14%,说明本方法准确可行。