固相萃取-液相色谱串联质谱法测定城市污水中他莫昔芬和来曲唑

他莫昔芬和来曲唑常用于治疗雌激素依赖型乳腺癌。本研究建立了城市污水中他莫昔芬和来曲唑的超高效液相色谱-串联质谱(UPLC-MS/MS)联用检测方法。水样通过Oasis HLB固相萃取柱富集后串联氨基柱,先用6 mL甲醇洗脱,再用3 mL甲醇洗脱氨基柱,合并洗脱液后浓缩。使用ACQUITY UPLCTM BEH C18反相柱,流动相为0.1%甲酸-乙腈,在梯度条件下分离;目标分析物使用超高效液相色谱-电喷雾串联质谱进行测定。本方法对他莫昔芬和来曲唑的线性范围分别是1.0～100μg/L和0.1～100μg/L,相关系数R2>0.997,检出限分别为1.0和0.1 ng/L,进水和出水的3个不同水平的加标平均回收率为68.8%～103.0%,相对标准偏差小于15%。本方法可用于城市污水中相关物质的分析。     

Self-Assembly of ZnII/CdII/PbII Coordination Polymers with a Tripodal Ligand Derived from Aromatase Inhibitor Letrozole Derivative

Reactions of the aromatase inhibitor letrozole derivative 4,4'-(1H-1,2,4-triazol-1-yl)methylene-bis(benzonic acid) (H₂tzmb) with Zn^II, Cd^II, or Pb^II salts under similar conditions resulted in the generation of three coordination polymers, namely, {[Zn(tzmb)(H₂tzmb)] · H₂O}_n ( 1 ), [Cd(tzmb)(H₂O)₂]_n ( 2 ), and {[Pb(tzmb)(H₂O)] · DMF}_n ( 3 ), respectively. Their structures were determined by single-crystal X-ray diffraction analyses and further characterized by elemental analysis, IR spectroscopy, powder X-ray diffraction, and thermogravimetric analyses. Complex 1 features a twofold 2D → 2D interpenetrated network based on corrugated 6³- hcb layers, and complex 2 exhibits a flat 2D 4.8²- fes network, whereas complex 3 presents a 3D hex net based on infinite rod-shaped secondary building units. The remarkable structural diversity may illustrate the powerful effect of metal ions on coordination assemblies. The spectroscopic, thermal, and photoluminescent properties of complexes 1 – 3 were investigated. In addition, the catalytic activity of 1 in the solvent-free ring-opening polymerization of ε-caprolactone was also discussed.     

Development and validation of an UHPLC-MS/MS method for simultaneous determination of palbociclib,letrozole and its metabolite carbinol in rat plasma and pharmacokinetic study application

A sensitive and selective UHPLC-MS/MS method was developed and validated to simultaneously determine of palbociclib (PLB), letrozole (LTZ) and its metabolite carbinol (CBL) in rat plasma. After sample pre-treatment by acetonitrile-protein precipitation, the chromatographies resolution was performed using a reversed phase Acquity® UPLC BEH C18 column (1.7 μm particle size, 50 mm × 2.1 mm ID) in isocratic mobile phase consisted of a mixture of methanol and water containing 0.1% acetic acid (55:45, v/v) at pH 4.5. The flow rate and run time were 300 µL/min and 2.5 min, respectively. The target drugs were detected in multiple reaction monitoring (MRM) mode using tandem mass spectrometer coupled to a positive ESI interface to monitor the precursor-to-product ion transitions. Method validation was assessed as per the FDA guidelines for determination of PLB, LTZ and CBL within the concentration ranges 0.5–600 ng/mL for PLB and LTZ and 0.2–200 ng/mL for CBL (r² ≥ 0.997). The rest of validation parameters were within the accepted limits. The validated method was applied to PK study of these drugs in rats, and succeeded to determine the values of the PK parameters of PLB and LTZ.     

Synthesis,Crystal Structure,and Characterization of three New Letrozole Complexes

Three new letrozole complexes {[Cu(Le)₄Cl₂] · (H₂O)} ( 1 ), {[Ni(Le)₄Cl₂] · (H₂O)}( 2 ) and {[Co(Le)₄Cl₂] · (H₂O)} ( 3 ) (Le = letrozole = 1‐[bis(4‐cyanophenyl)methyl]‐1, 2, 4‐triazole) were obtained from self‐assembly of CuCl₂, NiCl₂ · 6H₂O, and CoCl₂ · 6H₂O with medicine letrozole. All compounds were characterized by IR spectroscopy, elemental, single‐crystal as well as powder X‐ray diffraction, and thermogravimetric analyses. The analyses of the structures indicate that all crystals belong to monoclinic system, space group C2/c, for complex 1 with crystal data a = 34.501(18) Å, b = 12.724(7) Å, c = 16.116(9) Å, β = 114.958(7) °, V = 6414(6) Å ³, Z = 4, F(000) = 2660, R₁ = 0.0668, wR₂ = 0.1574; for complex 2 , a = 34.769(6) Å, b = 12.7267(18) Å, c = 16.046(2) Å, β = 115.281(3) °, V = 6420.1(16) Å ³, Z = 4, F(000) = 2656, R₁ = 0.0510, wR₂ = 0.0896; for complex 3 , a = 35.063(8) Å,b = 12.658(3) Å, c = 16.056(4) Å, β = 115.387(3) °, V = 6438(2) ų, Z = 4, F(000) = 2652, R₁ = 0.0528, wR₂ = 0.1205. The local arrangements around central metal atoms (Cu^II, Ni^II, and Co^II) can be best described as distorted octahedra which are constructed by two chlorine atoms and four monodentate nitrogen atoms from different letrozole ligands. XRD results of 1 – 3 show that all peaks displayed in the measured patterns at room temperature closely match those in the simulated patterns generated from single‐crystal diffraction data, indicating single phases of 1 – 3 were formed.     

紫外分光光度法测定抗癌药物来曲唑的含量

建立了紫外分光光度法测定药物来曲唑含量的方法。在乙腈溶液中,来曲唑的最大吸收波长在240 nm处,摩尔吸收系数为3.396×104L.mol-1.cm-1,来曲唑的浓度在2.89×10-6~2.31×10-5mol/L范围内吸光度与浓度呈良好的线性关系。该方法操作简单,重现性好,准确,用于来曲唑片剂含量的测定,结果满意。