高效液相色谱法测定红花中的羟基红花黄色素A

建立了菊科植物红花中的主要有效成分羟基红花黄色素A的高效液相色谱定量分析方法。用90 ℃水提取,以甲醇-0.5%磷酸水溶液(体积比为40∶60)为流动相,检测波长400 nm。该方法的最低检出限为4 ng (按S/N=3计)。在羟基红花黄色素A的质量浓度为0.04-0.40 g/L(相当于绝对进样量为0.8-8.0 μg)时线性良好,方法回收率高,重现性好。对26个不同产地和购买地的红花中的羟基红花黄色素A进行了测定,结果表明不同来源的红花中羟基红花黄色素A含量的差异较大。     

高效液相色谱法测定藏药萨热大鹏丸中羟基红花黄色素A

用反相高效液相色谱法测定藏药萨热大鹏丸中的羟基红花黄色素A。C18色谱柱(4.6 mm×250 mm,5μm);流动相:甲醇-0.05%H3PO4溶液,梯度洗脱;流速:1 mL/min;柱温25℃;检测波长为403 nm。羟基红花黄色素A在0.11136~0.94654μg的范围内呈线性关系,回归方程为y=2435.7402x-10.9502,r=0.9999;平均加样回收率为99.9%,RSD为0.3%。该方法可用于萨热大鹏丸中羟基红花黄色素A的测定。     

RP-HPLC测定十四味羚牛角丸中羟基红花黄色素A的含量

应用高效液相色谱的方法建立藏药十四味羚牛角丸中羟基红花黄色素A的定量分析.色谱条件:用Symmetry C18(5μm,4.6×250 mm);流动相:V(甲醇):V(水):V(H3PO4)=26:74:0.05,检测波长:403 nm,流速:1.0mL/min,羟基红花黄色素A在6～96μg/mL范围内呈良好线性关系,r=0.9996,十四味羚牛角丸中羟基红花黄色素A的回收率为99.24%(RSD=1.9%,n=5).本方法简便、快速、准确、灵敏度高、重现性好,可用于藏药十四味羚牛角丸中羟基红花黄色素A的含量测定.     

超高效液相色谱法测定新疆不同产地的红花中羟基红花黄色素A的含量北大核心CSCD

称取经粉碎的样品0.100 0g,加入10mL水,超声处理20min后,用水定容至25mL,过0.22μm有机滤膜后,在Thermo Hypersil Gold C18色谱柱(100mm×2.1mm,1.9μm)上分离,以乙腈-0.1%(体积分数)甲酸溶液为流动相进行梯度洗脱,采用二极管阵列检测器,检测波长为403nm。羟基红花黄色素A的质量浓度在42~336mg·L-1内与其峰面积呈线性关系,检出限(3S/N)为19.3μg·L^(-1)。加标回收率在92.7%~95.2%之间,测定值的相对标准偏差(n=6)小于1.0%。方法用于测定新疆不同产地的红花中羟基红花黄色素A的含量,测定值在24.00~46.43mg·g-1之间,聚类分析结果表明,红花药材样品可以聚为四大类。     

超高效液相色谱法同时测定红景天保健品中红景天苷和甙元酪醇含量

提出了超高效液相色谱法同时测定红景天保健品中红景天苷和甙元酪醇含量的方法.样品经甲醇超声提取,以Acquity UPLCTM BEH色谱柱(2.1 mm×50 mm,1.7 μm)为固定相,以磷酸(0.05+99.5)溶液-乙腈混合液为流动相作梯度淋洗,用二极管列阵检测器,检测波长为221.3 nm.红景天苷和甙元酪醇的质量在0.01～0.3 g·L-1范围内与其吸光度呈线性关系.应用此法测定红景天茎根和红景天胶囊,平均回收率在90.67%～95.55%和90.73%～96.52%之间.     

高效液相色谱法测定野菊花中蒙花苷的含量

建立高效液相色谱法测定野菊花中蒙花苷含量的方法。采用KromosilTM C18十八烷基硅烷键合硅胶色谱柱,甲醇-水-乙酸(体积比为55∶44.5∶0.5)为流动相,流速为0.8mL/min,柱温为室温,检测波长为334nm。蒙花苷含量在11.2~89.6μg/mL范围内,线性关系良好(r=0.9998),方法的相对标准偏差为0.51%(n=5),平均加标回收率为98.92%。     

高效液相色谱法测定环孢素A含量

提出了高效液相色谱法测定环孢素A含量的方法。以Agilent Extend C18色谱柱(250mm×4.6mm,5μm)为固定相,以乙腈、水、叔丁基甲醚和磷酸按体积比500比500比50比1的混合溶液为流动相,用紫外检测器检测,检测波长为210nm。环孢素A的质量浓度在0.025～2.00g.L-1范围内与其峰面积呈线性关系。方法应用于环孢素原料药分析,测定结果的相对标准偏差(n=6)小于1.0%,用标准加入法做回收试验,回收率在99.3%～101%之间。     

高效液相色谱法测定镇咳药中左旋羟基苯哌嗪含量

建立了高效液相色谱法(HPLC)测定镇咳药中左旋羟基苯哌嗪含量的方法,运用二极管阵列检测器(PAD),C18反相柱,以甲醇∶水(冰醋酸HAc调节pH值为6.5)∶三乙胺(TEA)(30∶70∶0.5,V/V/V),为流动相测定了3批镇咳药(利咳净糖浆)中左旋羟基苯哌嗪的含量分别为5772.65、809.25、833.2μg/mL,变异系数小于2%,回收率为99.1%~100.2%.该方法快速,精密度及准确度在允许范围内,可作为镇咳药中左旋羟基苯哌嗪的测定方法.     

高效液相色谱法测定苁蓉酒中松果菊苷的含量

建立反相高效液相色谱法测定苁蓉酒中松果菊苷含量。固定相为C18,流动相为甲醇-0．1％甲酸水溶液（体积比为33：67）,流速1．0mL／min,柱温为30℃,检测波长为330nm。松果菊苷的浓度x（mg／mL）与其峰高y呈良好的线性关系,线性方程为Y=2．5955x,相关系数为0．9999。样品的加标回收率为88．1％～107．5％,测定结果相对标准偏差为0．41％（n=5）。     

不同产地红景天药材中红景天甙含量的测定

以红景天甙含量为指标建立了红景天药材的HPLC定量分析方法.色谱条件:C18柱(250 mm×4.6 mm,25μm),甲醇-乙腈-水为流动相梯度洗脱,检测波长为275 nm.该法灵敏度高,重现性好.利用本方法对六种不同产地红景天药材中红景天甙的含量进行了分析比较.结果表明,产地不同,红景天甙的含量差别很大,其中以云南丽江地区产的含量最高.     

Determination of hydroxysafflor yellow A in rat plasma and tissues by high-performance liquid chromatography after oral administration of safflower extract or safflor yellow

A simple and reproducible HPLC method for quantification of hydroxysafflor yellow A (HSYA) in rat plasma and tissues after oral administration of safflower extract or safflor yellow (SY) was developed. Sample preparation was achieved by protein precipitation of plasma and tissue homogenates with three volumes of methanol. p-Hydroxybenzaldehyde was used as the internal standard (IS). HSYA and IS were separated on a Hypersil BDS-C(18) column with a gradient elution system composed of acetonitrile and aqueous acetic acid. UV detection was used at 320 nm. The calibration curves were linear in all matrices (r(2) > 0.999) in the concentration ranges 0.51-101.36 microg/mL for plasma, 12.27-2454.46 microg/g for intestines and 0.96-192.20 microg/g for lung. The intra-day and inter-day precision were all less than 12.5%, and the extract recovery was in the range 64.1-103.7% with RSD less than 15.6% for HSYA in all matrices. The method was used successfully to quantify HSYA in rat plasma and tissue samples to support a pharmacokinectic study.     

高效液相色谱法测定糕点中的柠檬黄、日落黄

建立高效液相色谱法测定糕点中的柠檬黄、日落黄的方法。样品经水浸泡提取,于涡旋混匀器中快速混匀,浸泡放置过夜,取离心后的上清液,以甲醇和乙酸铵溶液梯度淋洗,用紫外检测器检测,柠檬黄、日落黄分别采用430 nm和482 nm检测波长。线性相关系数为0.999,柠檬黄、日落黄的检出限分别为0.4,0.3 mg/kg。样品加标回收率为72.5%~82.0%,柠檬黄、日落黄测定结果的相对标准偏差分别为4.8%和3.7%(n=5)。方法简便快捷,节省试剂,减少了杂质干扰,提高了灵敏度。     

高效液相色谱法测定发酵液中杆菌肽A

提出了高效液相色谱法测定发酵液中杆菌肽A含量的方法。地衣芽孢杆菌发酵液经离心得到杆菌肽A的粗提液。所得粗提液再经三氯乙酸提取,离心分离。取上清液用Beckman C18色谱柱分离,用乙腈和磷酸二氢钾缓冲溶液以不同体积比混合为流动相梯度洗脱,在220 nm波长处进行测定。杆菌肽A的质量浓度在1.0~15.0 g·L-1范围内与其峰面积呈线性关系,检出限(3S/N)为0.08 g·L-1。在7.37 g·L-1和11.01 g·L-1两个添加水平做回收试验,平均回收率分别为98.1%和97.4%。     

高效液相色谱法测定竹节参中多种人参皂苷含量

建立了高效液相色谱法(HPLC)测定竹节参中人参皂苷Rg1、Re、Rb1、Rb2、Rg2、Rd含量的方法.运用二极管阵列检测器(DAD)峰纯度和光谱检索功能,结合保留时间定性,外标峰面积法定量.采用C18反相柱,以乙腈-水梯度洗脱测定了同一批竹节参总皂苷中人参皂苷Rg1、Re、Rd的含量分别为0.81%、0.15%、2.99%,回收率为93.46%~94.02%,含量及回收率的RSD均小于5%,该方法简便、灵敏,精密度及准确度在允许范围内,可作为竹节参皂苷提取物中多种人参皂苷的同时测定方法.     

高效液相色谱法测定打印油墨和色带中双酚A

提出了高效液相色谱法-二极管阵列检测器测定打印油墨和色带中双酚A含量的方法。采用正己烷-乙醚(30+70)溶液为提取溶剂,以XB-C18色谱柱为分离柱,以乙腈与甲酸(0.1+99.9)溶液按体积比40比60混合为流动相,流量1.0mL.min-1,检测波长为227nm。双酚A的质量浓度在0.34～10.96mg.L-1范围内与其峰面积呈线性关系,检出限(3S/N)为3.4μg.L-1。在3个浓度水平下做加标回收试验,回收率在89.8%～93.7%之间,相对标准偏差(n=7)在1.2%～2.5%之间。     

液液萃取/高效液相色谱法测定豆干与腐竹中溶剂黄2及溶剂黄56

建立了液液萃取/高效液相色谱法测定豆干和腐竹中溶剂黄2和溶剂黄56的分析方法。样品经乙腈饱和的正己烷提取后,加入正己烷饱和的乙腈萃取,将乙腈层转入浓缩瓶内,重复萃取3次,将萃取液浓缩后用乙腈定容。采用Agilent TC-C18(4.6 mm×250 mm,5μm)色谱柱对样品进行分离;柱温为30℃;流动相为水-甲醇(20∶80);流速为1.0 m L/min;检测波长为410 nm。溶剂黄2和溶剂黄56在0.30~50 mg/L浓度范围内线性关系良好,其检出限(LOD)和定量下限(LOQ)分别均为0.15 mg/kg和0.50 mg/kg,方法的平均回收率为85.4%~94.6%,相对标准偏差(RSD,n=6)为0.3%~2.3%。该方法重复性好,灵敏度高,适用于豆干和腐竹中溶剂黄2和溶剂黄56含量的测定。     

Determination of hydroxysafflor yellow A in biological fluids of patients with traumatic brain injury by UPLC‐ESI‐MS/MS after injection of Xuebijing

A simple, novel, specific, rapid and reproducible ultra‐performance liquid chromatography electrospray ionization tandem mass spectrometry method has been developed and validated for the determination of hydroxysafflor yellow A (HSYA) in biological fluids (plasma, urine and cerebrospinal fluid) of patients with traumatic brain injury after intravenous injection of Xuebijing (XBJ). Liquid–liquid extraction was performed, and separation was carried out on an Acquity UPLC? BEH C₁₈ column, with gradient elution using a mobile phase composed of methanol and 0.1% formic acid at a flow rate of 0.3 mL/min. A triple quadrupole tandem mass spectrometer with electrospray ionization was used for the detection of HSYA. The mass transition followed was m/z 611.0 → 491. The retention time was less than 3.0 min. The calibration curve was linear in the concentration range from 2 to 6125 ng/mL for cerebrospinal fluid, plasma and urine. The intra‐ and inter‐day precisions were <10%, and the relative standard deviation of recovery was <15% for HSYA in biological matrices. The method was successfully applied for the first time to quantify HSYA in the biological fluids (especially in cerebrospinal fluid) of patients with traumatic brain injury following intravenous administration of XBJ. Copyright © 2014 John Wiley & Sons, Ltd.     

Simultaneous determination of hydroxysafflor yellow A and ferulic acid in rat plasma after oral administration of the co-extractum of Rhizoma chuanxiong and Flos Carthami by HPLC-diode array detector

A simple, rapid and accurate HPLC method has been developed for simultaneous determination of hydroxysafflor yellow A and ferulic acid in rat plasma after oral administration of the co-extractum of Rhizoma chuanxiong and Flos Carthami. Plasma samples were deproteinized with 6% perchloric acid, and riboflavin was used as internal standard. The supernatant after centrifuge was injected into a Shimadzu C(18) (150 x 4.6 mm, i.d. 5 microm) column. Gradient elution for A:B (0 min, 90:10; 25 min, 70:30; 27 min, stop) was applied. The mobile phase was composed of 0.022 mol/L potassium dihydrogen phosphate solutions, adjusted to pH 3.0 with phosphoric acid for pump A, and 90% (v/v) acetonitrile for pump B. The assay was shown to be linear over the range 0.046-4.6 microg/mL (r(2) = 0.9995) for hydroxysafflor yellow A and 0.037-3.7 microg/mL (r(2) = 0.9998) for ferulic acid. Mean recovery was 97.5% for hydroxysafflor yellow A and 83.6% for ferulic acid. Both of the intra-day and inter-day precisions were 相似文献   

荧光光谱法测定饮料中的日落黄

建立了荧光光谱法测定饮料中日落黄含量的方法.实验结果表明,在pH为10的NH3·H2O-NH4Cl缓冲溶液中,日落黄在波长303 nm的紫外光激发下,最大发射波长位于430 nm,其荧光强度与日落黄浓度在0.05～4.0 mg/L范围内呈现良好的线性关系.方法的检出限(3σ)为0.024 mg/L,相对标准偏差(RSD...