RP-HPLC测定盐酸二甲双胍的血药浓度

目的建立用反相高效液相色谱法(RP-HPLC)测定人血浆样品中二甲双胍浓度的定量方法。方法应用Agilent1100系列高效液相色谱仪,AgilentZorbaxSB-C18色谱柱(5μm,150mm×4.6mm),流动相为0.01mol·L-1十二烷基硫酸钠-乙腈(63∶37,pH=4.0);检测波长233nm,流速1.0ml/min。结果盐酸二甲双胍浓度在0.06~4μg·ml-1范围内呈良好的线性关系(r=0.9997),平均回收率为(98.92±1.11)%,RSD为2.47%。结论RP-HPLC法简便、快捷、灵敏、准确,适用于临床药代动力学及药效学的研究。     

反相高效液相色谱法测定肾移植术后全血环孢素A浓度

目的建立单步萃取反相高效液相色谱法测定人全血中环孢素A(CsA)浓度。方法病人血样经乙醚单步萃取,环孢素D(CsD)为内标,C18色谱柱,乙腈-水(80:20)为流动相,流速1.0ml/min,柱温70℃,检测波长214nm。结果CsA全血浓度在50~600ng/ml范围内线性关系良好,r=0.9998,最低检测浓度为20ng/ml,平均回收率100.44%,日内和日间RSD均<5%。结论本法简便灵敏、准确可靠、经济,可用于临床人体器官移植术后全血中CsA浓度的监测。     

HPLC法测定桂龙咳喘宁颗粒中桂皮醛的含量

目的建立测定桂龙咳喘宁颗粒中桂皮醛的高效液相色谱法。方法采用高效液相色谱法,C18色谱柱(5μm,4.6mm×150mm);流动相:乙腈-0.1%磷酸(40∶60),流速1.0ml/min;检测波长285nm,外标一点法测定。结果线性范围4.2×10-5~21×10-5μg,r=0.9999。平均回收率为101.4%(RSD=1.2%,n=5)。结论建立了高效液相色谱法测定含量,准确、快速、重现性好。     

高效液相色谱法测定凝胶剂中地塞米松磷酸钠的含量

 目的 建立一种测定凝胶剂中地塞米松磷酸钠含量的高效液相色谱法.方法 采用反相高效液相色谱法,以Shim-pack vp-ODS柱(4.6 mm×150 mm,5 μm)做分析柱,以甲醇-0.025 mol/L KH2PO4缓冲液(60:40,V/V)为流动相,流速1.0 ml/min.柱箱温度50℃,苯甲酸为内标,检测波长为245 nm.结果 本法的日内精密度为RSD=0.35%,日间精密度为RSD=0.68%,平均回收率为100.4%.标准曲线在5～40 μg/ml浓度范围内,呈现良好的线性关系(r=0.9998).结论 该法用于地塞米松磷酸钠凝胶剂的含量测定,快速、准确、可行.     

HPLC法测定尿嘧啶替加氟片含量

目的采用HPLC法测定尿嘧啶替加氟片的含量。方法 Agilent1200 HPLC仪;Agilent ZOBAX C18色谱柱(150 mm×4.6 mm,5μm);流动相:甲醇-水(10∶90);流速:1.0 ml/min;柱温:30℃;检测波长:271 nm。结果尿嘧啶、替加氟分别在0.16～1.60μg、0.08～0.80μg范围内线性关系良好(r=0.9999、r=0.9995),平均加样回收率分别为99.53%、100.68%,RSD分别为0.74%、1.63%(n=6)。结论本方法简便、准确、重复性好,为完善本产品质量控制提供依据。     

反相离子对液相色谱法测定复方降压胶囊中磷酸氯喹含量的研究

目的　利用反相离子对液相色谱法测定复方降压胶囊中磷酸氯喹的含量。方法　采用HYPERSILODS2 (4 .6× 2 5 0mm ,5 μm)色谱柱 ,乙腈 -甲醇 -己烷磺酸钠溶液 (18∶18∶6 4 )为流动相 ,流速为 1.0ml/min ,检测波长 343nm。 结果　磷酸氯喹线性范围为 :2 1.6～ 2 81μg·ml-1,r=0 .9999;日内精密度 RSD 为 0 .4 2 % (n=6 ) ;日间精密度 RSD 为 0 .5 5 % (n=5 )。平均回收率为97.1% (n =9)。结论　本方法简便 ,准确 ,适用于该药的质量控制     

反相高效液相色谱法测定人血浆中替米沙坦的浓度

目的　建立RP -HPLC法测定人血浆中替米沙坦浓度。方法　用AgilentZORBAX×ODS柱 (4 .6× 1 5 0mm ,5 μm) ,流动相为水 -乙腈 -三乙胺 (6 0∶4 0∶0 .1 ) ,荧光检测激发波长为 30 0nm ,发射波长为 380nm ,采用萘乙酸为内标。结果　替米沙坦保留时间为 9min左右 ,浓度线性范围 1 0～ 35 0 0 μg·L-1 。结论　该法准确、快速、简便 ,可用作人血浆中替米沙坦浓度测定方法     

反相高效液相色谱法测定脑得生片中葛根素含量

报道RP-HPLC法测定脑得生片中葛根素含量。采用Shim-Pack CLC-ODS(15cm×6mmID)分析柱;北分厂ODS保护柱;流动相:甲醇-水(25:75);流速:1.0ml/min;色谱柱温度:35℃;ShimadzuFLD-6A荧光检测器(激发波长:350±20nm;检测波长450nm-800nm);进样体积10μl;外标法计算含量。理论塔板数按葛根素峰计算为2601,葛根素浓度在20μg/ml-120μg/ml范围与色谱峰面积呈线性关系,r=0.9998,平均回收率为99.46％,RSD1.5％。     

高效液相色谱法测定调经活血片中芍药苷的含量

 目的 建立HPLC法测定中成药调经活血片中芍药苷含量.方法 用WatersC18色谱柱.流动相为乙腈-0.05 mol/L磷酸二氢钾溶液(15∶85),流速为1.0 ml/min,检测波长为230 nm,柱温为25℃.结果 芍药苷在0.01～0.50 mg/ml浓度范围内与峰面积呈良好的线性关系(r=0.9999),平均回收率为98.84%,RSD为1.37%(n＝6).结论 该方法准确,灵敏度高,重现性好,可作为调经活血片的质量控制指标.     

RP-HPLC测定血浆中间硝苯地平的浓度

目的建立高效液相色谱法测定Beagle犬血浆中间硝苯地平(m-nifedipine,m-Nif)的浓度,并研究其代谢动力学规律。方法采用正交设计优选色谱和提取条件,血浆样品中m-Nif经碱化、萃取后,用反相高效液相色谱法(RP-HPLC)进行分析测定。色谱分析柱为C18柱(250mm×4.6mm,5μm);流动相为甲醇-10mmol·L-1磷酸盐缓冲液pH5(83∶17);流速为1.0ml/min;检测波长为350nm;内标为MN9201(二氢吡啶类)。结果线性范围为10~500ng·ml-1,最低检测浓度为10ng·ml-1,低、中、高3种不同浓度的方法回收率分别为110.84%、105.60%、104.23%;提取回收率分别为92.75%、104.46%、105.12%,日内RSD分别为9.70%、3.05%和1.75%;日间RSD分别为14.53%、7.21%和5.44%。结论本方法稳定、简便、准确,可用于Beagle犬血浆中m-Nif的浓度测定及药代动力学研究。     

HPLC法测定复方替米沙坦胶囊中替米沙坦和吲哒帕胺的含量

目的建立HPLC法同时测定复方替米沙坦胶囊中替米沙坦和吲哒帕胺的含量。方法采用Kromasil—ODS C18色谱柱,以乙腈．水．冰醋酸（45：55：0．1）为流动相,检测波长为242nm。替米沙坦、吲哒帕胺分别在50—150μg·ml^-1,r=0．9999;5～151μg·ml^-1,r=0．9998,浓度范围内线性关系良好。替米沙坦、吲哒帕胺的平均回收率分别为99．79％、99．64％,RSD分别为0．21％、0．81％。结果在选定的色谱条件下,替米沙坦和吲哒帕胺可以完全分离。结论方法准确,简便可靠,可作为复方替米沙坦胶囊的质量控制方法。     

HPLC法测定N393的含量

目的采用HPLC法测定N393的含量。方法选用迪马-C18（250mm×4.6mm,5μm）色谱柱,以乙腈-0.01mol.L-1磷酸二氢钾（KH2PO4）溶液（65∶35）为流动相,检测波长：220nm。结果N393在6～280μg·mL-1（r=0.9997）范围内线性关系良好,方法平均回收率为99.72%,RSD为0.67%（n=9）。结论本法可用于测定N393的含量。     

Prediction of a Large ASE Effect in Silver Plasmas Produced by a Short-Pulse-Drive Laser

A Ne-like laser scheme is considered for a pure silver plasma. Level populations and gain coefficients are calculated with an atomic-kinetics model. It is shown that large gain values (GL>100) are achievable in a hot dense quasi-steady-state silver plasma at λ=10.038 nm (2-1 transition) and λ=12.298 nm (0-1 transition). Lasing is also possible at λ=2.75 nm (2s-2p transition). The plasma conditions needed are: electron temperature 3?5& keV and density 5 × 1022 < ne < 1023;cm-3;. These plasma conditions can be created with a high-contrast, high-intensity short-pulse visible light laser driver.     

多潘立酮片人体药代动力学和生物等效性

目的研究多潘立酮片(湖南威特)在健康人体内的相对生物利用度和生物等效性,为新药报批及其临床应用提供依据。方法18名健康受试者采用随机双交叉试验方法,单剂量口服受试及参比制剂20 mg,用HPLC法测定给药后不同时间的血药浓度,计算主要药代动力学参数。结果受试制剂多潘立酮片(湖南威特)的T1/2:(9.31±1.60)h、Cmax:(27.2±2.5)μg/L、Tmax:(0.76±0.20)h、AUC0-t:(142.5±24.4)μg.h/L;参比制剂多潘立酮片(西安杨森)T1/2:(8.72±1.39)h、Cmax:(28.1±3.9)μg/L、Tmax:(0.78±0.21)h、AUC0-t:(140.9±27.3)μg.h/L。以AUC0-t计算,与参比制剂相比受试制剂中多潘立酮的平均相对生物利用度为(101.6%±5.1%)。结论两制剂生物等效。     

Chemoembolization of Hepatocellular Carcinoma with Hepasphere 30–60 μm. Safety and Efficacy Study

Background

This study examined the safety, pharmacokinetics, and efficacy of transarterial chemoembolization of hepatocellular carcinoma (HCC) using a newly developed size of a superabsorbent polymer drug-eluting embolic material.

Methods

Forty-five patients with documented HCC (Child–Pugh score A/B: 55.5 %/44.5 %) were embolized with HepaSphere microspheres 30–60 μm with escalation of lesion, dose, and frequency of re-embolization. Local response was evaluated with modified response evaluation criteria in solid tumors (mRECIST). Plasma levels of doxorubicin were measured in 24 patients at baseline and at 5, 20, 40, 60, and 120 min, at 6, 24, and 48 h, and at 7 days, respectively, to determine doxorubicin in plasma (Cmax) and area under the curve (AUC). Measurements of three patients who underwent lipiodol-based conventional chemoembolization (c-TACE) were also performed.

Results

TACE with HepaSphere was well tolerated with an acceptable safety profile and no 30-day mortality. Response rates were calculated on intention-to-treat basis with complete response (CR) in 17.8 % reaching 22.2 % for the target lesion. Overall partial response (PR) was seen in 51.1 %, stable disease in 20 %, and progressive disease in 11.1 % of patients. Overall objective response (CR + PR), including patients treated at all dosages of doxorubicin, was seen in 68.9 % of cases. After a median follow-up of 15.6 months, 1-year survival is 100 %. Doxorubicin AUC was significantly lower in patients with HepaSphere 30–60 μm (35,195 ± 27,873 ng × min/ml) than in patients with conventional TACE (103,960 ± 16,652 ng × min/ml; p = 0.009). Cmax was also significantly lower with HepaSphere 30–60 μm (83.9 ± 32.1 ng/ml) compared with c-TACE (761.3 ± 58.8 ng/ml; p = 0.002).

Conclusion

HepaSphere 30–60 μm is an effective drug-eluting embolic material with a favourable pharmacokinetic profile.     

文拉法辛的人体药代动力学

目的建立HPLC-荧光法测定人血浆中文拉法辛浓度,研究其在中国健康人体内的药代动力学。方法以Diamonsil C18（150mm×4．6mm,5um）为色谱柱;流动相为乙腈-磷酸盐缓冲液（pH3．0）．三乙胺（33．5：66．5：1,V/V／V）;流速1．0ml／min;进样量：20．0ul,内标为马普替林。血浆样品经正己烷．异戊醇提取,荧光检测条件：λex276nm,λem596nm。结果文拉法辛在10．0—800．0ng·ml^-1浓度范围内线性关系良好（r=0．9999）,最低血药检测浓度为16．99ng·ml^-1。文拉法辛浓度30．0,150．0,600．0ng·ml^-1的萃取回收率和相对回收率分别在81．51％-91．08％、98．7％-112．6％范围内,日内和日间精密度的RSD分别小于12％和10％（n=5）。文拉法辛的主要药动学参数：t1／2（6．57±2．81）h,Tmax（3．11±0．93）h,Cmax（273．38±75．44）ng·ml^-1,AUC（0-1）（2237．54±816．67）ng·h·ml^-1,AUC（0-∞）（2456．13±838．30）ng·h·ml^-1。结论HPLC-荧光法灵敏、准确、重复性好,适合于文拉法辛的临床药动学研究。     

HPLC测定四季红药材中槲皮素的含量

目的建立中药材四季红中槲皮素的HPLC含量测定方法。方法色谱柱为Hypersil BDS C18色谱柱（4．6mm×200mm,5μm）,流动相为甲醇-水-磷酸（50：50：0．4,V／V／V）,检测波长370nm。结果槲皮素在0．04～0．16μg的范围内呈良好线性关系（r=0．9998）,平均加样回收率为101．17％,RSD为1．42％（n=9）。结论本方法简便,准确,灵敏度高,重复性好,能有效测定四季红药材中槲皮素含量,为四季红的质量评价提供科学依据。     

Mutation Induction and RBE-LET Relationship of Low-energy Protons in V79 Cells

Summary

The mutation induction at the HGPRT locus has been studied in V79-753B Chinese hamster cells irradiated with proton beams with energies of 3·36, 1·70 and 1·16 MeV, corresponding to average LET values of 10·6, 17·8 and 23·9 keV/μm, respectively. The mutation curve obtained with 200 kV X-rays was used for comparison. The mutation frequency induced by all the proton beams is considerably higher than that induced at the same dose by X-rays and it is linearly related to the dose. Moreover, the proton effectiveness increases with the LET. The RBEs (evaluated as the initial slope ratios) are 5·0 ± 0·8, 5·4 ± 0·8 and 7·7 ± 1·2 for protons with average LETs of 10·6, 17·8 and 23·9 keV/μm, respectively. These values are higher than those reported in the literature for other ions of comparable LET. This finding parallels what we have already found for cell inactivation (for which RBEs of 3·0, 4·6 and 7·3 were obtained at the same LETs), and indicates that for mutation induction, also, the RBE-LET relationship may depend on the type of radiation.     

Dosimetric comparison of helical tomotherapy and VMAT for anal cancer: A single institutional experience

To compare the dosimetric results of helical tomotherapy (HT) and volumetric arc therapy (VMAT) in the treatment of anal cancer. Plans were created for 20 (n = 20) patients treated for anal cancer using HT and 2 arc VMAT. Dosimetric comparison was assessed for doses to targets and organs at risk (small bowel, bladder, external genitalia, and femoral heads). Delivery time and dosimetric verification results were also compared. HT showed a higher V95% for both primary and nodal targets (V95% increase by 0.5% to 1.3%; p = ≤0.05). No differences were seen in V105%, V107%, or V110 % between techniques. HT provided better sparing of the small bowel for dose levels V30, V35, and V40 (p = 0.005, 0.001, and 0.030), but was similar at higher doses. Similarly HT provided better bladder dose at V35 only (p = 0.020). Doses to femoral heads and genitalia were similar. Delivery time was higher for the HT plans (4.58 ± 1.1 min) than VMAT (3.13 ± 0.2 minutes) (p = 0.011). Dose verification results were 99.5 ± 0.9% and 100 ± 0% (HT, n = 6) vs 95.0 ± 3.1% and 99.2 ± 0.8% (VMAT, n = 20) for global gamma criteria 3%/3 mm and 4%/4 mm, respectively. Both HT and VMAT produced high quality plans that frequently met most of the dose objectives apart from genitalia V20, V40, bladder V35, and V50. Although absolute dose differences were small, the PTV V95%, small bowel V30, V35, and V40 and bladder V35 were statistically better in the HT plans. VMAT provided a shorter delivery time by 1.45 minutes; however, our HT plans were more likely to pass tighter plan dose verification criteria than VMAT.     

Letter to the Editor

The relative biological effectiveness (RBE) of selected low-LET radiation modalities (55 kVp X-rays, 250 kVp X-rays, ⁶⁰Co γ-rays, and 11 MeV electrons) was investigated for survival of two cell lines (V79 and CHO). Detailed measurements were made in the low (0 to 3 Gy) dose range using an image cytometry device to accurately determine the number of cells assayed at each dose point. Data were also collected in the high dose range (0 to 10 Gy) using conventional counting and plating techniques. RBE values (± 1 SE) varied from 1·0 ± 0·07 (V79 cells) and 1·2 ± 0·05 (CHO cells) at high doses to 1·3 ± 0·07 (V79) and 1·4 ± 0·1 (CHO) at low doses for 55 kVp X-rays, from 1·1 ± 0·05 (V79) and 1·1 ± 0·04 (CHO) at high doses to 1·1 ± 0·06 (V79) and 1·2 ± 0·2 (CHO) at low doses for 250 kVp X-rays, and from 1·1 ± 0·08 (V79) and 1·0 ± 0·04 (CHO) at high doses to 1·0 ± 0·06 (V79) and 0·9 ± 0·1 (CHO) at low doses for 11 MeV electrons. Only the low and high dose RBEs for 55 kVp X-rays relative to ⁶⁰Co γ-rays were significantly different.