反相高效液相色谱法同时测定化妆品中的16种激素

糖皮质激素对皮肤具有一定的嫩白作用,短时间使用含有糖皮质激素的化妆品可使皮肤光滑细腻、红润白嫩,有着较好的美容效果。但长期使用糖皮质激素,通过皮肤的吸收可引起全身的副作用,导致面部皮肤损害、骨质疏松、肌肉萎缩、生长发育迟缓、诱发或加重感染和消化性溃疡、情绪异常、代谢紊乱等各种不良反应。化妆品中添加雌激素、雄激素、孕激素等性激素能够在短时间内促进毛发生长,防止皮肤老化,有除皱、增加皮肤弹性等作用。但长久使用会导致色素沉积、产生黑斑、皮肤萎缩变薄,甚至具有致癌性,引发细胞癌、乳腺癌、卵巢癌等疾病。我国《化妆品卫乍标准》、《化妆品卫生规范》和欧盟化妆品规程（Directive 76／768／EEU）中均明确规定,糖皮质激素、雌激素、雄激素、孕激素等激素为化妆品组分中禁用物质。化妆品中激素的检验对于严格控制化妆品的产品质量,确保化妆品的使用安全,保障人民身体健康具有重要的意义。     

反相高效液相色谱法测定六味地黄软胶囊中的熊果酸

1引言六味地黄软胶囊与六味地黄丸的配方、功效与主治相同,即由山莱美、牡丹皮等六味药精制而成,具有滋阴补肾之功能,用于肾明亏损,头晕耳鸣,腰膝酸软,骨蒸潮热,盗汗遗精,消渴。熊果酸存在于山茱萸、山植、沙棘等多种中草药中,它具有强心、降脂、降糖、抗菌、抗炎、抗癌等生理活性,有着重要的药用价值。其测定方法主要有比色法和薄层扫描法;近几年又报道了高效液相色谱法,然而在中药制剂中未见报道,究其原因主要是制剂中成分复杂,干扰大。本文建立了六味地黄软胶囊中熊果酸的高效液相色谱测定法：以乙醚为提取溶剂,甲醇萃取…     

快速高效液相色谱法测定卷烟主流烟气中的酚

简单酚类化合物是卷烟主流烟气中的一类重要有害成分,采用液相色谱分离检测酚类化合物已有许多文献报道。为了进一步缩短分离时间,我们采用快速高效液相色谱法（HPLC）测定了卷烟主流烟气中的酚,主要酚在2．0min内可达到基线分离,取得令人满意的结果。     

反相高效液相色谱法测定朱砂根中的朱砂根皂苷

建立了朱砂根中朱砂根皂苷的反相高效液相色谱分析方法。采用SHIM-PACK VP-ODS色谱柱(250 mm×4.6 mm,5 μm),流动相为乙腈-水(体积比为37∶63),流速1.0 mL/min,检测波长205 nm,柱温40 ℃。朱砂根皂苷的进样量为144 ng～57.6 μg时线性关系良好(r=0.9997);加标回收率(n=3)为94.2%～99.4%,相对标准偏差为0.5%～2.0%。方法简便,准确性高,重复性好,适用于朱砂根中朱砂根皂苷的测定。     

反相高效液相色谱法测定泼尼松龙磷酸钠原料药及其注射液

泼尼松龙磷酸钠（prednisolone sodium phosphate,PPNa）为11β,17α,21-三羟基孕甾-1,4-二烯-3,20-二酮-21-磷酸酯二钠盐。目前国内还未上市销售,也无其分析方法的报道,但有对醋酸泼尼松龙进行分析的报道。美国药典26对其提取分离后用紫外分光光度法检测PPNa中的游离泼尼松龙,但对其注射液未做有关物质的测定;英国药典2002年版采用高效液相色谱法检测PPNa原料中的有关物质,流动相系统复杂。本文建立的反相高效液相色谱法。流动相系统简单。能将供试品中的主峰与杂质峰完全分离,方法快速灵敏、准确度高、重复性好,可用于PPNa原料药及其注射剂的含量测定和有关物质的测定。     

反相高效液相色谱法测定合成产物中的双酚芴

建立了采用反相高效液相色谱测定合成的双酚芴含量的方法。采用反相C18烷基柱,以甲醇-水（体积比为85∶15）为流动相,流速为1.0 mL/min,采用UVD170紫外检测器在230 nm处进行检测。双酚芴质量浓度为4～20 mg/L时,其峰面积与质量浓度的线性关系良好,线性相关系数为0.9996;平均回收率高于98.7%,相对标准偏差低于1%。结果表明,所建立的方法简单快速、准确可靠。     

非水反相高效液相色谱法测定阿立哌唑的含量

阿立哌唑(aripiprazole,7-[4-[4-(2,3-二氯苯基)-1-哌嗪基]-丁氧基]-3,4-二氢化喹喏啉酮)是日本Otsuka公司于1988年开发的第二代非典型性抗精神病药,于2002年由美国食品药品管理局(FDA)批准上市,商品名为Abilify,用于精神分裂症的治疗[1]。阿立哌唑的含量测定方法尚未见报道。1     

十二烷基糖苷的反相高效液相色谱分析

烷基多苷（APG）是一类环保型非离子表面活性剂,由脂肪醇与糖制备,为单糖苷和多糖苷的混合物.受分离方法的限制,难以得到其中各组分的纯品,因此APG的组成测定一直未得到很好的解决.本文采用制备色谱对其进行分离,经核磁共振氢谱（^1H NMR）确定各组分的结构,用高效液相色谱（HPLC）分析测定了相对质量校正因子（f）,为完善APG的结构分析及质量控制奠定了基础.     

反相高效液相色谱法同时测定化妆品中的9种糖皮质激素

建立了化妆品中9种糖皮质激素的反相高效液相(RP-HPLC)测定方法.采用酸化甲醇振荡提取,HLB固相萃取小柱净化,HPLC分离测定.在定量范围内均呈良好的线性关系(r≥0.999);回收率为85.0%～99.5%,相对标准偏差小于5.8%,检出限(LOD) (S/N≥3)为1.0 ng,定量限(LOQ) (S/N≥10)为2.0 ng.该法可用于化妆品中泼尼松龙、氢化可的松、可的松、甲基强的松龙、地塞米松、氟米松、倍氯米松、曲安奈德和氟轻松的检测.     

反相高效液相色谱法测定化妆品中L-抗坏血酸磷酸镁含量

L-抗坏血酸磷酸镁(AS-PM)用在化妆品中作增白剂和抗辐射剂。AS-PM是极性分子,通常使用一个阴离子交换柱进行色谱分离,本文用四氢呋喃。磷酸盐缓冲溶液溶解稀释化妆品样品后,在氨丙基柱上以乙腈一磷酸盐缓冲溶液为流动相测定其中的AS-PM。     

Two new taraxerane-type triterpenes from Ledum palustre L.

Abstract

Two new compounds, namely 6α-hydroxy-14-taraxerene-3,16,21-trione and 6α,26-dihydroxy-14-taraxerene-3,16,21-trione were isolated from the Ledum palustre L. Their chemical structures were confirmed after a combined analysis of IR, HR-ESI-TOFMS, 1D-NMR, and 2D-NMR. The compounds were evaluated for cell growth inhibitory activity against two cancer cell lines.     

Chemical composition of Ledum palustre

Summary Extraction of the herbLedum palustre with liquefied carbon dioxide and Khladon-11 has yielded 10 individual substances belonging to various classes and various groups of organic compounds: hydrocarbons, alcohols, ketones, monoterpenes, sesquiterpenes, and flavonoids.All-Union Scientific-Research Institute of Medicinal Plants, Moscow. Translated from Khimiya Prirodnykh Soedinenii, No. 1, pp. 127–130, January–February, 1978.     

反相高效液相色谱法测定银杏中银杏酸

采用反相高效液相色谱法测定银杏中5种银杏酸的含量。样品用甲醇为提取溶剂回流提取后定容至25 mL,取2 mL用正己烷从含有硅藻土的pH 2～3溶液进行液-液萃取,上清液真空旋干,加甲醇定容至2 mL后,取20μL进样用Waters Symmetry-C₁₈色谱柱分离,以甲醇-水（88+12,含5%乙酸）为流动相,二极管阵列检测器在波长310 nm处检测。峰面积与5种银杏酸的质量浓度分别在一定范围内呈线性关系,方法的检出限（3S/N）在0.26～1.37 mg·L^-1之间。方法的平均回收率为99.2%,测定值的相对标准偏差（n=5）为6.83%。     

大兴安岭地区细叶杜香挥发性成分的研究

1　实验部分1.1　仪器与样品　　固相微萃取(SPME)手柄及100μm聚二甲基硅氧烷(PDMS)萃取头(美国Supelco),恒温磁力搅拌装置,GC 17A QP5050GC/MS仪(日本Shimadzu)。　　细叶杜香2002年8月采于内蒙古大兴安岭,在避光处将其自然晾干后,将其嫩枝和叶剪成细末,待用。1.2　杜香挥发性成分的提取　　水蒸气蒸馏:取细叶杜香样品100g,按常规方法进行水蒸气蒸馏,提取6h,水层用氯化钠饱和后,用乙醚萃取,回收乙醚,得棕黄色透明油状物0 6g,将其用乙醚稀释后用于气相色谱 质谱(GC/MS)分析。　　SPME:将SPME纤维在GC/MS仪进样口250℃下老化2…     

New terpenoids of the essential oil of Ledum palustre

The structures of two new natural compounds isolated from the essential oil ofLedum palustre L. have been established on the basis of their spectral characteristics as p-mentha-1,8(10)-diene 3,9-epoxide (lepaloks) and 3,10-epoxygermacr-4(14)-en-8-one (lepakson). The chemical structure of ledene as a sesquiterpene hydrocarbon has been determined by chemical correlation.Tomsk State Medical Institute. Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR, Novosibirsk. Translated from Khimiya Prirodnykh Soedinenii, No. 1, pp. 24–29, January–February, 1991.     

Bicyclic monoterpenoids of the essential oil of Ledum palustre

The structure of a new natural compound has been established as 5-isopropylbicyclo[3.1.0]hex-3-en-2-one, which has been called lebaikon. Two bicyclic monoterpenoids (2-formyl-5-isopropylbicyclo[3.1.0]hex-2-ene and 4-isopropyl-1-methylbicyclo[3.1.0]hexan-2-one) have been detected in natural materials for the first time.     

Bicyclic monoterpenoids of the essential oil of Ledum palustre

The structure of a new natural compound has been established as 5-isopropylbicyclo[3.1.0]hex-3-en-2-one, which has been called lebaikon. Two bicyclic monoterpenoids (2-formyl-5-isopropylbicyclo[3.1.0]hex-2-ene and 4-isopropyl-1-methylbicyclo[3.1.0]hexan-2-one) have been detected in natural materials for the first time.Tomsk State Medical Institute. Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR, Novosibirsk. Translated from Khimiya Prirodnykh Soedinenii, No. 5, pp. 627–629, September–October, 1990.     

Intraspecies chemical variability of the essential oil of Ledum palustre

The compositions of the essential oils of marsh tea,Ledum palustre L., from the southern regions of Tomsk, Transbaikalia and Amur province, and also from the southern part of the island of Sakhalin have been analyzed in detail. The results obtained indicate the sharply pronounced intraspecies chemical variability of this plant. In addition to the chemotype of march tea with myrcene as a macrocomponent which is widely distributed in the European part of the USSR, another three chemotypes with the macrocomponents limonene, sabinen, and p-cymene have been revealed.Tomsk State Medical Institute. Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodnykh Soedinenii, No. 4, pp. 472–480, July–August, 1990.