Determination of Benzo[a]pyrene in Edible Oil by High Performance Liquid Chromatography-Fluorescence Detector (HPLC-FL)

In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Scientific C18 column (250 mm×4.6 mm, 5 μm) as the chromatographic column and acetonitrile and water as the mobile phase, and the excitation wavelength and emission wavelength of fluorescence detector were 286 and 430 nm, respectively. The response was high, and the linear range was 0.5-10.0 ng/ml. The lowest limit of detection was 0.11 ng/ml, and the average recovery was 92.5%. This method is suitable for quantitative analysis of benzo[a]pyrene content in edible oil.

Determination of AF and AFG in Red Ginseng by High Performance Liquid Chromatography with Evaporative Light Scattering Detector (HPLC-ELSD)

[Objective]The paper was to establish a method for determining AF and AFG in red ginseng.[Method]A new simple,rapid and sensitive method for simultaneous determination of two amadori compounds,arginyl-fructose(AF)and arginyl-fructosyl-glucose(AFG),in extracts of three kinds of ginseng preparations was developed and validated using high performance liquid chromatography with evaporative light scattering detector(HPLC-ELSD).Two target analytes were efficiently separated by Prevail CTM18 column(4.6 mm×250 mm,5μm)at the flow rate of 0.8 mL/min within 15 min of single chromatographic run.[Result]Under optimized conditions,the detection limits were 0.015 and 0.02 mg/mL for AF and AFG,respectively.Calibration curves of peak area for two analytes were linear over three orders of magnitude with the correlation coefficients greater than 0.999.The average recoveries,precision,reproducibility and stability for two analytes(AF and AFG)were 99.5% and 100.9%,0.43% and 0.47%,0.46% and 0.43%,0.41% and 0.49%,respectively.[Conclusion]This method was successfully applied for quantifying AF and AFG in red ginseng and the method was efficient,sensitive and accurate.

Research Advances in Detection Techniques of High Performance Liquid Chromatography-Refractive Index Detector

As a highly sensitive and stable detector,refractive index detector is usually used for quantitative detection of substances such as polymer,sugar and organic acid. The research reviewed the application of HPLC-RID in the fields of quantitative determination of medicine and food,in order to lay a foundation for wider use of RID.

Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography coupled with diode array detector and evaporative light scattering detector

A simple and accurate high-performance liquid chromatography（HPLC）coupled with diode array detector（DAD）and evaporative light scattering detector（ELSD）was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation（ZFP）.The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis（HCA）,which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.

Simultaneous Determination of Saponins in Radix Glycyrrhizae, Notoginseng and Ginseng by High Performance Liquid Chromatography

To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liquid chromatography with diode array detector(HPLC-DAD) method was applied to an Inertsil ODS-SP column(4.6 mm×250 mm, 5 μm) with a mobile phase consisting of acetonitrile-0.05% phosphoric acid in a gradient elution manner. The flow rate was 1.0 mL/min. The column temperature was 30 ℃ and the detection wavelengths were 203 nm and 237 nm, respectively. The linear ranges were 0.700,0—7.000,0 μg for R1(r=1.000,0), 0.751,1— 7.511,4 μg for Rg1(r=1.000,0), 0.677,2—6.771,6 μg for Re(r=1.000,0), 0.733,9—7.339,1 μg for Rb1(r= 1.000,0), and 0.540,0—5.399,8 μg for ammonium glycyrrhizinate(r=0.999,9), respectively. In addition, their average recoveries were 100.28%, 105.83%, 104.09%, 99.36% and 98.54%, respectively. The relative standard deviations(RSDs) of precision, reproducibility and recovery were all less than 1.5%. The results indicate that the method is simple, accurate and reproducible so that it can be used for the simultaneous determination of the five saponins in Chinese patent medicines containing the three kinds of herbs.

Fast determination of tobramycin by reversed-phase ion-pair high performance liquid chromatography with a refractive index detector

A simple and direct method without a deriva- tion step for routine analysis of tobramycin has been developed. This method used reversed-phase ion-pair high performance liquid chromatography （HPLC） with a refractive index （RI） detector and a C18 column which is stable at pH above 1.00. The presence of 4.50mg.mL ] trifluoroacetic acid （TFA） in the mobile phase improved the protonation of tobramycin and the formation of ionpairs, and thus reduced its hydrophility. This unique separation-detection combination showed good linearity with correlation coefficients 0.9996 in the concentration range of 0.25-2.50mg.mL 1. The quantitation limit and detection limit were determined to be 0.23 mg.mL ~ and 0.071 mg. mL ~, respectively. Tobramycin was recovered in 98.00%, 98.84% and 99.64% for tobramycin solutions at concentrations of 2.25 mg.mL^-1, 1.50mg.mL 1 and 0.75 mg.mL ＇, respectively. The relative standard deviations for six spiked samples ranged from 0.20% to 2.40%, indicating a good reproducibility of this method.

HPLC-PDA法测定明日叶不同部位中的4-羟基德里辛和黄色当归醇含量

采用高效液相色谱配备光电二极管阵列检测器法测定明日叶根、茎和叶中4-羟基德里辛（4-hydroxyderricin,4-HD）和黄色当归醇（xanthoangelol,XAG）的含量。样品分析选用Halo C（18）色谱柱（4.6 mm×150 mm,2.7μm）,流动相为0.1%甲酸（A）-甲醇（B）溶液,梯度洗脱,流速为0.3 m L/min,检测波长为370 nm,柱温为40℃。4-HD、XAG在0.945-18.900、1.048-20.960μg/m L质量浓度范围内线性关系良好,样品含量的相对标准偏差分别为3.13%、2.52%,方法的重复性好,平均回收率分别为103.70%、103.05%。经检测明日叶中4-HD的分布规律为：茎（149.16μg/g）〉根（122.42μg/g）〉叶（1.24μg/g）;XAG的分布规律为：根（144.28μg/g）〉茎（75.17μg/g）〉叶（1.21μg/g）。4-HD和XAG在根和茎中的分布显著高于其在叶中的分布。

HPLC-PDA-MS快速测定“染红食品”中苏丹红残留量方法的研究

[目的]建立“染红食品”中苏丹红Ⅰ、Ⅱ、Ⅲ和Ⅳ残留量的高效液相色谱(HPLC)初筛、质谱确认分析方法。[方法]以Merck RP-18柱为分析柱,流动相:乙腈∶水=90∶10,Waters-2996二极管矩阵检测器(PDA)和FinniganLCQ Deca XP MAX质谱仪为检测器。[结果]回归方程和相关系数为:苏丹红Ⅰ:y=0.163104x+0.019217,r=0.99993;苏丹红Ⅱ:y=0.153674x-0.2212981,r=0.99993;苏丹红Ⅲ:y=0.305919x-5.0810264,r=0.9997;苏丹红Ⅳ:y=0.239273x-5.260669,r=0.9997。平均回收率(%):87.3、83.0、86.7和90.0。[结论]用HPLC-PDA-MS法检测食品中的苏丹红方法简便,重现性好,灵敏度高,定性准确,定量精确。

高效液相色谱法测定α-烯基磺酸盐中的磺内酯

建立了高效液相色谱法测定α-烯基磺酸盐中磺内酯的定量分析方法,并用该方法对市售4批α-烯基磺酸盐样品进行风险监测。样品经水和乙醇溶解,溶解后用石油醚萃取。萃取物溶于正己烷与异丙醇的混合溶液中。采用高效液相色谱法,以正己烷和异丙醇为流动相进行等度洗脱。二者体积比8∶2,流速为2.0 mL/min,Inertsil CN-3柱(250 mm×4.6 mm×5μm)色谱柱分离,进样量为20μL,柱温为25℃。检测器为蒸发光散射检测器。漂移管温度为80℃,载气流速为2.0 L/min。外标法定量。结果显示:磺内酯在80~200μg/mL质量浓度范围内呈良好线性关系,检出限为5.25μg/mL,相关系数大于0.989,相对标准偏差为1.01%(n=6)。磺内酯的加标回收率为102.82%~108.24%。该方法分离效果好,线性关系好,操作简便,灵敏度高,准确度和重复性好。该方法能快速、准确地测定α-烯基磺酸盐中磺内酯的残留量。

乙腈盐析萃取HPLC-PDA同时测定水中11种苯胺类化合物

通过对色谱分析和样品萃取条件的选择和优化，建立了同时分析水中11种苯胺类化合物的HPLC方法。样品经乙腈盐析萃取后直接进样分析，采用ODS色谱柱，以乙腈-水为流动相进行梯度洗脱，用PDA检测。结果表明，11种苯胺类化合物在0．20—100mg／L范围内其浓度和检测信号呈良好的线性关系，方法检出限为0．002～0．007mg／L，地表水和废水样品加标回收率为81．6％～97．4％，相对标准偏差为1．5％～5．5％。

动物源食品中四环素、土霉素、盐酸克伦特罗HPLC-PDA同时快速检测方法的研究

[目的 ]建立动物源性食品中抗生素、盐酸克伦特罗的高效液相色谱 (HPLC)分析方法。 [方法 ]以WatersNova PakC184μm柱为分析柱 ,Na2 HPO4∶乙晴为 75∶2 5 ,Waters 2 695二极管矩阵检测器 (PDA)为检测器。 [结果 ]线性回归方程和相关系数为 :土霉素 y =0 5 5 0 0 7x -0 0 0 4176,r =0 99980 ;四环素y =0 5 945x + 0 0 2 764 ,r =0 9998;盐酸克伦特罗 y =0 0 14 3 5x + 0 0 2 63 46,r =0 9975。平均回收率为 93 82 5 %、93 760 %和 94 745 %。[结论 ]HPLC PDA法同时检测动物源性食品中的土霉素、四环素和盐酸克伦特罗 ,定性准确 。

HPLC-PDA法同时测定羽裂蟹甲草花中3种香豆素的含量

目的建立能同时测定羽裂蟹甲草花中7-羟基香豆素(HC)、7-羟基-8-甲氧基香豆素(HMC)和7β-D-葡萄糖-8-羟基香豆素(GC)含量的高效液相色谱-二极管阵列检测器(HPLC-PDA)法。方法采用Kromasil C 18色谱柱(250 mm×4.6 mm,5μm),以甲醇-四氢呋喃-10 mL·L^(-1)醋酸(27∶7∶66)为流动相;流速:0.8 mL·min^(-1);检测波长:325 nm。结果HC、HMC和GC质量浓度分别在1~120、1~120、2~120μg·mL^(-1)范围内与峰面积呈良好的线性关系,相关系数分别为0.9998、0.9998、0.9999;平均回收率分别为101.92%、98.47%、98.94%。结论所建立的方法简便、快速、准确,可用于羽裂蟹甲草花的质量控制,并为香豆素类化合物的分离分析提供参考。

ASE-UPLC-PDA法测定PM_(2.5)中16种多环芳烃

采用二极管阵列检测器（PDA）,建立了加速溶剂萃取（ASE）-超高效液相色谱（UPLC）定性定量测定大气PM2.5中16种多环芳烃（PAHs）的方法。通过优化预处理过程及柱温、梯度洗脱程序等一系列色谱分离条件,实现了14 min内16种PAHs的完全基线分离。优化条件下测定PAHs线性关系好,检出限为0.50-2.0μg/L,样品加标回收率为75%-98%,相对标准偏差为0.54%-8.97%。结果表明,该方法用于测定大气PM2.5中PAHs的含量,具有检出限低、灵敏度高、重复性好等优点,是一个较为可靠的检测方法。

SPE-HPLC联用PDA/FLD串联分析污水厂中的PAHs

以测定城镇污水厂中多环芳烃（PAils）为背景，探讨SPE-HPLC联用PDA／FLD双检测器串联分析方法。利用4因素3水平正交实验得出固相萃取最佳条件，先利用过硅胶柱对萃取液进行净化，然后利用HPLC的PDA／FLD双串联检测器分析了污水水样中16种PAHs。峰面积与浓度有良好的线性关系，相关系数〉0．999，检出限为0．1～35ng／L，加标回收率〉95．25％，相对标准偏差（RSD）为0．68％～9．0％。将方法应用于济南光大水务污水厂进、出水中PAHs的测定，其总浓度分别为24．07μg／L和1．75μg／L，污水处理厂对PAHs的综合去除率为92．70％，加标回收率为87．65％～93．28％。该方法操作简单、灵敏度高，适于复杂水体中PAHs的检测。

HPLC-PDA法检验保健食品中的盐酸西布曲明

目的：以紫外检测器检测，根据色谱峰的绝对保留时间定性，对可疑阳性样品二极管阵列检测器再定性，用外标法峰面积定量，建立保健食品中盐酸西布曲明的测定方法。方法：采用反相高效液相色谱法，Symmetry C18（4．6×250mm，5μm）色谱柱，流动相为甲醇-水-三乙胺（75：25：0．1），流速为1．0ml／min，检测波长为223nm.结果：其工作曲线的线性范围：10—200μg／ml，相关系数：r=0．9999，回收率：97．07％，RSD：1．39％。结论：方法准确、可靠，可用于保健品中盐酸西布曲明的检测。

HPLC Analysis of Egg Yolk Phosphatidylcholine by Evaporative Light Scattering Detector

Egg yolk phosphatidylcholine(EYPC) is being widely used in food and pharmaceutical industries nowadays owing to its surface activity,pharmaceutical usefulness,and so on.Common determination methods of phospholipids were based on the American Oil Chemists' Society(AOCS) Official Method Ja7b-91,in which n-hexane/2-propanol/acetate buffer was used as the mobile phase.In order to achieve desired results,gradient elu-tion or buffer solution was used,which made the detection process more complicated.Moreover,water or buffer solution could affect the silica gel column both on its lifespan and the separation efficiency significantly.In this study,different mobile phase and detector were used to simplify EYPC analyzing process instead of using water within the mobile phase.The optimized HPLC operating conditions are as follows:pure methanol as a mobile phase,flow rate of 1.0 ml·min-1,silica gel column(250 mm×4.6 mm,5 μm,Inertsil GLTM),column temperature 30 ℃ and low temperature evaporative light scattering detector(40 ℃,0.35 MPa) as used.Under this optimal condition,the linear relative coefficient of the standard curve is 0.998 and the recovery was in the range of 96.83%-101.58% with a relative standard deviation of 1.79%(n=6).

Study on chromatographic fingerprint of sarcandra glabra (Thunb.) by microwave-assisted extraction coupled to HPLC/DAD

Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chromatography/diode array detector(HPLC/DAD).The conditions of MAE were optimized by an orthogonal experiment,and then the authentication and validation of the chromatographic fingerprint were conducted.Nine peaks were identified as common peaks in the fingerprint chromatograms,and isofraxidin was considered as a reference compound and quantified.Relative standard deviations of retention time and peak area of each component were less than 3% and 8%,respectively.Similarity and difference analysis were conducted by use of PCA and relation coefficient.Twenty batches of sarcandra glabra(Thunb.)samples from two different producing areas could be classified into two different groups in the PCA model.The results showed that MAE-HPLC/DAD method was simple,efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra(Thunb.),which could provide more reliable and precise information for quality evaluation.

Phytochemical Analysis of Ziziphus jujuba Leaves in Six Cultivars at the Whole Life Stage by High Performance Liquid Chromatography

Leaves of Ziziphus jujuba Mill.（Z. jujuba） were used as a folk medicine to treat children suffering from typhoid fever, furuncle and ecthyma in China. The present study was to establish a high performance liquid chroma- tography-diode array detector（HPLC-DAD） method for quality control of Z. jujuba leaves. The validated method was applied to the simultaneous characterization and quantification of sixteen main constituents in thirty samples, which comprised the whole life stage of Z. ]ujuba leaves from six cultivars in Yulin, Shannxi Province, China. HPLC fin- gerprint file of Z. jujuba leaves was set up and the results indicate that the major constituents of Z. jujuba leaves are （-）-catechin（1）, quercetin-3-O-robinobioside（3）, rutin（4） and quercetin-3-O-a-L-arabinosyl-（1---~2）-a-L-rhamnoside（6） with the total contents of the nine flavonoids in respective batch ranging from 18.52 mg/g to 39.51 mg/g. In addition, the contents of compounds depend on both the season and the cultivar. During ripening of Z. jujuba leaves, flavo- noids of all the cultivars present a similar trend： initially decrease from 25th, Jun. to 5th, Aug., 2015, and then in- crease for a period of time, finally slightly fluctuate on 5th Oct. The highest contents of total flavonoids were regis- tered on 25th Jun., 2015. Different cultivars have 50%--90% variation on the content for the three classes of com- pounds. Taken together, the results demonstrate that Z. jujuba leaves have great potential to be a new health-promoting resource based on flavonoids and the best sampling time of them is in June.

HPLC-PDA法同时测定金嗓子喉片中没食子酸和绿原酸的含量

目的:建立了一种同时测定金嗓子喉片中没食子酸和绿原酸含量的二极管阵列检测器色谱(HPLC-PDA)方法。方法:采用资生堂C18色谱柱(4. 6 mm×250 mm,5μm),以乙腈-0. 1%磷酸水为流动相进行梯度洗脱,流速为1. 0 mL·min^(-1),柱温为25℃,检测波长设为270 nm(没食子酸)和330 nm(绿原酸)。结果:没食子酸与绿原酸浓度分别在10. 02～80. 16μg·mL^(-1)(r=0. 999 8)和5. 973～47. 78μg·mL^(-1)(r=0. 999 7)范围内与峰面积呈良好的线性关系,平均回收率分别为100. 3%(RSD=0. 59%)和99. 6%(RSD=0. 85%),待测液在室温的条件下,60 h之内保持稳定。结论:本方法专属性强,重复性好,结果准确,可用于金嗓子喉片中没食子酸、绿原酸的含量测定。

丹磺酰肼衍生-高效液相色谱-荧光检测器法测定水中痕量3-羟基丙醛

提出了丹磺酰肼衍生-高效液相色谱-荧光检测器法测定水中痕量3-羟基丙醛(3-HPA)的方法。将1.0 g水样、2.0 mL含200 mg·L^(-1)丹磺酰肼的乙腈溶液、1.0 mL 3.0%(体积分数)乙酸溶液混合,再用乙腈定容至50 mL,于40℃衍生反应30 min。以Agilent Eclipse Plus C_(18)色谱柱为固定相,以不同体积比的乙腈-0.10%(质量分数)七氟丁酸溶液的混合溶液为流动相进行梯度洗脱,采用荧光检测器测定。结果表明:衍生试剂丹磺酰肼与3-HPA衍生物在20 min内可实现基线分离;3-HPA的质量浓度在7.6~380.0μg·L^(-1)内与衍生物的峰面积呈线性关系,检出限(3S/N)为1.1μg·L^(-1);方法用于实际水样分析,测定值的相对标准偏差(n=6)为0.71%,3-HPA的加标回收率为98.0%~102%。