Milli q plus system

Acetonitrile (HPLC super gradient grade) and methanol (HPLC super gradient grade) were purchased from Lab-Scan (Dublin, Ireland). Hydrochloric acid p.a. (36.5%) was a product of Ultrapure water produced by a Milli-Q Plus system (Millipore Corporation, Burlington, MA, USA). The AccQ•TagReagent Kit was purchased from Waters (Milford, MA, USA). The reagent kit consists of Waters AccQ•Fluor Borate Buffer, Waters AccQ•Fluor Reagent Powder (6-aminoquinolyl-N-hydroxy-succinimidyl carbamate—AQC), Waters AccQ•Fluor Reagent Diluent, Waters AccQ•Tag Amino Acid Analyzing Column (Nova-Pak C18, 4 µL, 150 × 3.9 mm), and Waters Amino Acid Hydrolysate Standard (each ampoule contains a 2.5 mM mixture of the 17 hydrolysate amino acids except for cystine—1.25 mM), i.e., aspartic acid (Asp), serine (Ser), glutamic acid (Glu), glycine (Gly), histidine (His), arginine (Arg), threonine (Thr), alanine (Ala), proline (Pro), cysteine (Cys), tyrosine (Tyr), valine (Val), methionine (Met), lysine (Lys), isoleucine (Ile), leucine (Leu), and phenylalanine (Phe)).

Samples of Ophiopogon japonicus were collected from the Sichuan and Zhejiang provinces of China. Samples of Liriope spicata var. prolifera were collected from the Hubei province of China. The detailed sample information was listed in Table 5. The botanical origin of materials was identified by the corresponding author. The voucher specimens (CMD-1~CMD-14, ZMD-1~ZMD-8 and SMD-1~SMD-4) were deposited at the Institute of Chinese Medical Sciences, University of Macau, Macao SAR, China.
The reference standards of ophiopojaponin C, ophiopogonin D, liriopesides B, ophiopognin D’, methylophiopogonone A, methylophiopogonone B, methylophiopogonanone A, methylophiopogonanone B and ruscogenin were purchased from Baoji Herbest Bio-Tech Co., Ltd. (Baoji, China). Anhydrous ethanol was purchased from Fuyu Fine Chemical Co., Ltd. (Tianjin, China). HPLC grade acetonitrile was purchased from Merck (Darmstadt, Germany). A2780 human ovarian cancer cell line was purchased from KeyGEN BioTECH Ltd. (Jiangsu, China). DMEM medium, fetal bovine serum (FBS), penicillin and streptomycin were purchased from Gibco, Thermo Fisher Scientific (Waltham, MA, USA). Dimethyl sulfoxide (DMSO), 3-(4, 5-Dimethylthiazol-2-yl)-2, 5-diphenyl tetrazolium bromide (MTT) were purchased from Sigma (St. Louis, MO, USA). Deionized water was prepared by Millipore Milli Q-Plus system (Billerica, MA, USA).

Lipid nanocapsules were made of Labrafac Lipophile WL 1349 (caprylic/capric triglyceride), Phospholipon 90G (soybean lecithin at 97.1% of phosphatidylcholine), and Solutol HS15 (a mixture of free polyethylene glycol 660 and polyethylene glycol 660 hydroxystearate) generously provided by Gattefosse S.A.S. (Saint-Priest, France), Phospholipid GmbH (Köln, Germany), and Laserson (Etampes, France), respectively. Deionized water was obtained from a Milli-Q plus system (Millipore, Paris, France). WS12 from Tocris (Lille, France), DiI, other chemical reagents and solvents were obtained from Sigma-Aldrich (Saint-Quentin Fallavier, France) and used as received.

Glu (98%, lot no. 140690-200401) was purchased from National Standard Material Centre (Beijing, China); Homoserine (IS) (99%, lot no. 5005F23A) was purchased from Alfa Aesar Chemical Co. Ltd (Shanghai, China); Gln (99%, lot no. BCBH4247V), GABA (97%, lot no. BCBN4574V), o-phthalaldehyde (OPA), β-mercaptoethanol, disodium hydrogen phosphate, sodium borate and perchloric acid were purchased from Sigma Aldrich Chemie (Steinheim, Germany). HPLC-grade acetonitrile and methanol were purchased from Merck (Darmstadt, Germany). Water was purified by means of a Milli-Q plus system from Millipore (Bedford, MA).

Compound dexamethasone acetate cream (DXA) was obtained from China Resources Sanjiu Medical and Pharmaceutical Co., Ltd. (Shenzhen, China). Imiquimod cream was purchased from Sichuan Mingxin Pharmaceutical Co., Ltd. (Sichuan, China). P. granatum peels were obtained from fruit purchased from Kangmei Pharmaceutical Co., Ltd. (Guangdong, China). The enhanced chemiluminescence (ECL) reagent was obtained from Millipore (Billerica, MA, USA). d-Fucose (Fuc), d-xylose (Xyl), d-galacturonic acid (GalA), d-galactose (Gal), d-glucose (Glc), d-mannose (Man), l-rhamnose (Rha), d-arabinose (Ara), d-glucuronic acid (GlcA), and d-fructose (Fru) were obtained from Sigma (St. Louis, MO, USA). Deionized water was prepared using a Millipore MilliQ Plus system (Millipore, Bedford, MA, USA). All the other reagents were of analytical grade.

All solvents were purchased from Sigma-Aldrich (Taufkirchen, Germany). Water was purified by a Milli-Qplus system from Millipore (Milford, MA, USA). Sephadex LH-20 was purchased from Sigma-Aldrich. Nylon filters (0.45 µm pore size) were from Agilent (Agilent Technologies, Palo Alto, CA, USA).

The pure solution of RTX was Truxima^® (10 g/L, Celltrion Healthcare, Budapest, Hungary) for LC-MS/HRMS assay and Rixathon^® (10 g/L, Sandoz, Kundl, Austria) for LC-MS/MS assay. Full-length stable isotope-labeled rituximab (Arginine 13C6-15N4 and Lysine 13C6-15N2) (SIL-RTX) was purchased from Promise Advanced Proteomics (Grenoble, France). SIL-RTX presented with a purity > 95% and labeling > 99%. Stock solutions of RTX and SIL-RTX were prepared in water at 1 g/L and at 100 mg/L, respectively, and stored at +4 °C.
ULC/MS grade acetonitrile was obtained from Biosolve (Dieuze, France) and formic acid (FA) from Fisher Chemicals (Illkirch, France). Ultrapure water (resistivity 18.2 mΩ.cm) was obtained using a Milli-Q Plus^® system (Millipore, Molsheim, France). PBS buffer (pH 7.4, molarity 10X) was from Gibco (Thermo Fisher, Waltham, MA, USA). Trypsin Gold, Mass Spectrometry Grade were purchased from Promega (Madison, WI, USA). Propan-2-ol for analysis and trichloroacetic acid 20% for analysis were obtained from Carlo Erba Reagents (Val-de-Reuil, France). Ammonium bicarbonate for mass spectrometry was from Sigma-Aldrich (Saint-Quentin-Fallavier, France). Drug-free human plasma was provided by the regional blood service (EFS Rhône-Alpes and Ile-de-France, France). Low adsorption polypropylene microtubes from Dutsher (Brumath, France) were used throughout the study.