CWA Analytical Methods: Contaminants of Emerging Concern
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Pharmaceuticals and Personal Care Products (PPCPs) Methods Development
The EPA has developed two analytical methods to identify and measure certain contaminants of emerging concern, specifically:
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Method 1694 for a suite of 74 pharmaceuticals and personal care products
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Method 1698 for a suite of 27 steroids and hormones, that may be determined in wastewater effluents and influents, and sewage sludge (biosolids)
These methods were validated in a single laboratory, and initially published in 2007. They have not undergone multi-laboratory validation, and have not been approved for NPDES compliance monitoring purposes at 40 CFR Part 136. Method 1694 is a compilation of at least four procedures with different extractions and analysis conditions. Since 2007, many laboratories have successfully implemented these methods or modified versions.
| Number | Method Title |
|---|---|
| 1694 | Pharmaceuticals and Personal Care Products in Water, Soil, Sediment, and Biosolids by HPLC/MS/MS (2007) |
| 1698 | Steroids and Hormones in Water, Soil, Sediment, and Biosolids by HRGC/HRMS (2007) |
Contaminants of Emerging Concern in EPA Methods 1694 and 1698
| PPCP | CAS # | Classification |
|---|---|---|
| Acetaminophen | 103-90-2 | Antipyretic, analgesic |
| Albuterol | 18559-94-9 | Antiasthmatic |
| Ampicillin | 69-53-4 | β-lactam antibiotics |
| Anhydrochlortetracycline (ACTC) | 13803-65-1 | Chlorotetracycline degradate |
| Anhydrotetracycline (ATC) | 4496-85-9 | Chlorotetracycline degradate |
| Azithromycin | 83905-01-5 | Macrolide antibiotic |
| Caffeine | 58-08-2 | Stimulant |
| Carbadox | 6804 07 05 | Quinoxaline antibiotic |
| Carbamazepine | 298-46-4 | Anticonvulsant |
| Cefotaxime | 63527-52-6 | Cephalosporin antibiotic |
| Chlortetracycline (CTC) | 57-62-5 | Tetracycline antibiotic |
| Cimetidine | 51481-61-9 | Anti-acid reflux |
| Ciprofloxacin | 85721-33-1 | Quinoline antibiotic |
| Clarithromycin | 81103-11-9 | Macrolide antibiotic |
| Clinafloxacin | 105956-97-6 | Quinoline antibiotic |
| Cloxacillin | 61-72-3 | β-lactam antibiotics |
| Codeine | 76-57-3 | Opiate |
| Cotinine | 486-56-6 | Nicotine metabolite |
| Dehydronifedipine | 67035-22-7 | Nifedipine metabolite |
| Demeclocycline | 127-33-3 | Tetracycline antibiotic |
| Digoxigenin | 1672-46-4 | Immunohistochemical marker steroid |
| Digoxin | 20830-75-5 | Cardiac glycoside |
| Diltiazem | 42399-41-7 | Antihypertensive |
| 1,7-Dimethylxanthine | 611-59-6 | Antispasmodic, caffeine metabolite |
| Diphenhydramine | 58-73-1 | Antihistamine |
| Doxycycline | 564-25-0 | Tetracycline antibiotic |
| Enrofloxacin | 93106-60-6 | Quinolone antibiotic |
| 4-Epianhydrochlortetracycline (EACTC) | 158018-53-2 | Chlorotetracycline degradate |
| 4-Epianhydrotetracycline (EATC) | 4465-65-0 | Chlorotetracycline degradate |
| 4-Epichlortetracycline (ECTC) | 14297-93-9 | Chlorotetracycline degradate |
| 4-Epioxytetracycline (EOTC) | 14206-58-7 | Oxytetracycline degradate |
| 4-Epitetracycline (ETC) | 23313-80-6 | Tetracycline degradate |
| Erythromycin | 114-07-8 | Macrolide antibiotic |
| Erythromycin anhydrate | 59319-72-1 | Macrolide antibiotic |
| Flumequine | 42835-25-6 | Quinolone antibiotic |
| Fluoxetine | 54910-89-3 | SSRI antidepressant |
| Gemfibrozil | 25812-30-0 | Antilipemic |
| Ibuprofen | 15687-27-1 | Analgesic |
| Isochlortetracycline (ICTC) | 514-53-4 | Chlorotetracycline degradate |
| Lincomycin | 154-21-2 | Lincosamide antibiotic |
| Lomefloxacin | 98079-51-7 | Quinoline antibiotic |
| Metformin | 657-24-9 | Anti-diabetes drug |
| Miconazole | 22916-47-8 | Antifungal agent |
| Minocycline | 10118-91-8 | Tetracycline antibiotic |
| Naproxen | 22204-53-1 | Non-steroidal anti-inflammatory drug |
| Norfloxacin | 70458-96-7 | Quinoline antibiotic |
| Norgestimate | 35189-28-7 | Hormonal contraceptives |
| Ofloxacin | 82419-36-1 | Quinoline antibiotic |
| Ormetoprim | 6981-18-6 | Macrolide antibiotic |
| Oxacillin | 66-79-5 | β-lactam antibiotics |
| Oxolinic acid | 14698-29-4 | Quinolone antibiotic |
| Oxytetracycline (OTC) | 79-57-2 | Tetracycline antibiotic |
| Penicillin G | 61-33-6 | β-lactam antibiotics |
| Penicillin V | 87-08-1 | β-lactam antibiotics |
| Ranitidine | 66357-35-5 | Anti-acid reflux |
| Roxithromycin | 80214-83-1 | Macrolide antibiotic |
| Sarafloxacin | 98105-99-8 | Fluoroquinolone antibiotic |
| Sulfachloropyridazine | 80-32-0 | Sulfonamide antibiotic |
| Sulfadiazine | 68-35-9 | Sulfonamide antibiotic |
| Sulfadimethoxine | 122-11-2 | Sulfonamide antibiotic |
| Sulfamerazine | 127-79-7 | Sulfonamide antibiotic |
| Sulfamethazine | 57-68-1 | Sulfonamide antibiotic |
| Sulfamethizole | 144-82-1 | Sulfonamide antibiotic |
| Sulfamethoxazole | 723-46-6 | Sulfonamide antibiotic |
| Sulfanilamide | 63-74-1 | Sulfonamide antibiotic |
| Sulfathiazole | 72-14-0 | Sulfonamide antibiotic |
| Tetracycline (TC) | 60-54-8 | Tetracycline antibiotic |
| Thiabendazole | 148-79-8 | Fungicide and parasiticide |
| Triclocarban | 101-20-2 | Antimicrobial, disinfectant |
| Triclosan | 3380-34-5 | Antimicrobial, disinfectant |
| Trimethoprim | 738-70-5 | Pyrimidine antibiotic |
| Tylosin | 1401-69-0 | Macrolide antibiotic |
| Virginiamycin | 11006-76-1 | Macrolide antibiotic |
| Warfarin | 81-81-2 | Anticoagulant |
| Steroid/Hormone | CAS # | Classification |
|---|---|---|
| Androstenedione | 63-05-8 | anabolic agent |
| Androsterone | 53-41-8 | hormone metabolite |
| Equilenin | 517-09-9 | hormone replacement |
| Equilin | 474-86-2 | hormone replacement |
| 17a-Ethynyl Estradiol (EE2) | 57-63-6 | ovulation inhibitor |
| Desogestrel | 54024-22-5 | ovulation inhibitor |
| Mestranol | 72-33-3 | ovulation inhibitor |
| Norethindrone | 68-22-4 | ovulation inhibitor |
| Norgestrel | 6533-00-2 | ovulation inhibitor |
| Campesterol | 474-62-4 | Phytosterol (plant sterol) |
| beta-Sitosterol | 83-46-5 | Phytosterol (plant sterol) |
| Stigmasterol | 83-48-7 | Phytosterol (plant sterol) |
| Beta-Stigmastanol | 83-45-4 | Phytosterol (plant sterol) |
| 17a-Estradiol | 57-91-0 | Sex Hormone |
| 17b-Estradiol (E2) | 50-28-2 | Sex Hormone |
| Estriol (E3) | 50-27-1 | Sex Hormone |
| Estrone (E1) | 53-16-7 | Sex Hormone |
| Progesterone | 57-83-0 | Sex Hormone |
| Testosterone | 58-22-0 | Sex Hormone |
| 17a-Dihydroequilin | 651-55-8 | Sterol |
| Cholestanol | 80-97-7 | Sterol |
| Cholesterol | 57-88-5 | Sterol |
| Desmosterol | 313-04-2 | Sterol |
| Ergosterol | 57-87-4 | Sterol |
| b-Estradiol-3-benzoate | 50-50-0 | Sterol |
| Coprostanol | 360-68-9 | Sterol |
| Epi-Coprostanol | 516-92-7 | Sterol |
Other New Methods
The EPA also has developed and single lab validated Method 1614A, a revised version of the high-resolution GC/MS procedure for the polybrominated diphenyl ethers (PBDEs) used as flame retardants and Method 1699, a new high-resolution GC/MS method for organochlorine pesticides.
| Number | Method Title |
|---|---|
| 1614A | Brominated Diphenyl Ethers in Water Soil, Sediment and Tissue by HRGC/HRMS (2010) |
| 1699 | Pesticides in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS (2007) |
These methods have been validated in a single laboratory and peer-reviewed. The PBDEs in Method 1614A are not currently regulated, and while many of the pesticides in Method 1699 are regulated, neither of these methods have been promulgated at 40 CFR Part 136.